CN108752031A - A kind of method that carbon fiber prepares large-size carbon carbon crucible - Google Patents

A kind of method that carbon fiber prepares large-size carbon carbon crucible Download PDF

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CN108752031A
CN108752031A CN201810600329.XA CN201810600329A CN108752031A CN 108752031 A CN108752031 A CN 108752031A CN 201810600329 A CN201810600329 A CN 201810600329A CN 108752031 A CN108752031 A CN 108752031A
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carbon
crucible
gas
temperature
prepared
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朱瑞源
贾纮
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New Northwest Carbon Element Science And Technology Ltd In Gansu
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New Northwest Carbon Element Science And Technology Ltd In Gansu
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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    • 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
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
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    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6567—Treatment time
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    • 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
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/658—Atmosphere during thermal treatment
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/95—Products characterised by their size, e.g. microceramics
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • C04B2235/963—Surface properties, e.g. surface roughness

Abstract

The present invention relates to C-base composte material fields,More particularly to being a kind of method that carbon fiber prepares large-size carbon carbon crucible,First two kinds of carbon fibers is selected to be interleaved,It is prepared into prefabricated component,Prefabricated component is completed into infiltration molding by CVI densifications again,It is prepared into molded part,Then molded part is placed into heating furnace,Vacuumize heating,Surface of shaped parts pressure is passed through argon gas to normal pressure after being -0.08mpa,Molded part is taken out in blow-on,Molded part is prepared into the single piece of crucible shape by mechanical processing again,Outer surface is polished by single piece by polishing machine again,It is prepared into polished part,Finally polished part is placed into gaseous phase deposition stove,Vacuumize heating,After reaching temperature,It is passed through propane and argon gas is deposited,Continue to vacuumize after deposition,It stands,Blow-on,Take out carbon carbon crucible,In the preparation for solving existing carbon carbon crucible,There are difficulty for the molding of large scale graphite product,Reliability reduces,It is more difficult to be suitable for the problem of above carbon carbon crucible of 26 inch is processed.

Description

A kind of method that carbon fiber prepares large-size carbon carbon crucible
Technical field
The present invention relates to C-base composte material fields, and in particular to is the side that a kind of carbon fiber prepares large-size carbon carbon crucible Method.
Background technology
It is considered as in photovoltaic industry, semiconductor applications as heat structure part, heat-barrier material using C-base composte material The new stage of equal applications and a higher technology developing stage.Carbon/carbon compound material is carbon fiber reinforced carbon matrix bluk recombination Material, with light weight, ablation resistance is good, thermal-shock resistance is good, damage tolerance is high, elevated temperature strength is high, designability is strong etc. Outstanding feature, therefore, it has wide application in many fields such as space flight, aviation, atomic energy.And composite material can lead to Type, structure, quantity and matrix precursor and the process conditions of selection fiber are crossed to prepare required by meeting special-purpose Performance and shape, therefore it will be used wider and wider general, also increasingly be valued by people.Carbon/carbon compound material intensity It is far longer than graphite, good stability of the dimension, impact resistance, thermal shock resistance are good, and comprehensive mechanical performance is better than graphite.
With the demand of client, the increase of silicon material batch brings the specification of crucible also gradually to increase（Turned by 22,24 inch For 26 inch even bigger）.There are the increase of the cost of graphite crucible and the molding of large scale graphite product, there are difficulty, reliabilities The problem of reduction.
Chinese patent " monoblock type carbon carbon crucible and its manufacturing method ", application publication number CN106245117A disclose one The preparation method of kind of carbon carbon crucible, mainly solve carbon carbon crucible can only single-piece deposition, superposition can not be further continued for place to carry out The problem of deposition, has some limitations, it is more difficult to be suitable for the above carbon carbon crucible processing of 26 inch.
Therefore it needs one kind on the basis of existing equipment, does not do big change, yield rate and crystal forming rate can be improved, reduce Process costs, improve shaping efficiency, a kind of carbon fiber for preparing large-size carbon carbon crucible prepares large-size carbon carbon crucible Method.
Invention content
The present invention is in the preparation of existing carbon carbon crucible, and there are difficulty, reliability drops for the molding of large scale graphite product It is low, it is more difficult to which that the problem of being suitable for the above carbon carbon crucible processing of 26 inch provides the side that a kind of carbon fiber prepares large-size carbon carbon crucible Method.
The present invention solves above-mentioned technical problem, the technical solution adopted is that, a kind of carbon fiber prepares large-size carbon carbon crucible Method, include the following steps：
The first step, woven fabric select T700 12K carbon fibers and T700 6K carbon fibers, two kinds of carbon fibers are interleaved, are prepared into Prefabricated component；
Prefabricated component is completed infiltration molding by CVI densifications, is prepared into molded part by second step, material molding；
Third walks, and molded part is placed into heating furnace by high-temperature heat treatment, vacuumizes heating, surface of shaped parts pressure for- Argon gas is passed through after 0.08mpa to normal pressure, molded part is taken out in blow-on；
Molded part is prepared into the single piece of crucible shape by mechanical processing, then single piece is led to by the 4th step, processing, polishing It crosses polishing machine to be polished outer surface, is prepared into polished part；
Polished part is placed into gaseous phase deposition stove by the 5th step, surface coated treatment, vacuumizes heating, after reaching temperature, is passed through Propane and argon gas are deposited, and continue to vacuumize after deposition, are stood, blow-on, and carbon carbon crucible is taken out.
The purpose designed in this way is, carries out woven fabric using T700 12K carbon fibers and T700 6K carbon fibers, can improve The mechanical strength of integral material prevents cracked in following process or the phenomenon that burst.
Meanwhile the processing scheme being combined using CVI and CVD, CVI, that is, Chemical Vapor Infiltrationization Learn gas-phase permeation, reactant gas can be penetrated into inside precast body, occur chemically react simultaneously is deposited, make prefabricated component at Type.
Using CVD, that is, chemical vapor deposition chemical vapor depositions, to entire work piece surface into Row coating treatment is allowed to after the size for increasing carbon carbon crucible, and entire crucible internal performance and external performance can meet needs, In the preparation for solving existing carbon carbon crucible, there are difficulty, reliability reduces, it is more difficult to be suitable for for the molding of large scale graphite product The problem of above carbon carbon crucible of 26 inch is processed.
Further, the first step, woven fabric carry out T700 12K carbon fibers and T700 6K carbon fibers as basic material Interweave, and the texture that interweaves is plain weave.
The purpose designed in this way is, can be substantially without the intertexture through weft yarn by using the interleaving mode of plain weave Improve its mechanical strength so that entire yarn arrangement is even closer.
Further, second step, material molding, prefabricated component is placed into gas-phase permeation stove, is vacuumized, and keeps pressure, It heats up again and keeps temperature in CVI infiltration stoves, be passed through propane gas, permeated.
Optionally, second step, material molding, it is 4~10KPa to vacuumize pressure in rear gas-phase permeation stove, when keeping pressure Between be 0.5~1h, heating parameter be temperature in the gas-phase permeation stove in vacuum to be first promoted to 800 DEG C, and keep 0.5h, Temperature in the gas-phase permeation stove in vacuum is promoted to 1300 DEG C from 800 DEG C again, propane gas is passed through after 6~8h, makes gas phase Pressure falls to 1~2KPa in infiltration stove, keeps 80h.
The purpose designed in this way is, by carrying out more gradient-heateds after gas-phase permeation stove evacuation, being allowed to carbon carbon fiber Applied stress between dimension can be released, and improve the durable performance of integral material.
Further, third walks, and high-temperature heat treatment, heating parameters are that furnace temp is promoted to 1000 DEG C from room temperature, Temperature increase rate is 100 DEG C/h~300 DEG C/h, furnace temp is then promoted to 2000 DEG C from 1000 DEG C, temperature is promoted Rate is 50 DEG C/h~150 DEG C/h, then furnace temp is promoted to 2500 DEG C from 2000 DEG C, and temperature increase rate is 30 DEG C/h ~70 DEG C/h, finally heated furnace temperature is maintained at 2500 DEG C, 3~5h.
The purpose designed in this way is, when carrying out high-temperature process, carries out more gradient-heateds, the work being allowed between carbon carbon fiber It can be released with stress, improve the durable performance of integral material.
Optionally, the 4th step, processing, polishing, polishing degree are 0.1 μm of Ra <.
Further, the 5th step, surface coated treatment, after polished part is placed into gaseous phase deposition stove evacuation, gas phase is heavy Shallow lake furnace pressure is 4~10KPa, and heating parameters are gaseous phase deposition in-furnace temperature to be promoted to 1200 ± 100 DEG C from room temperature, so It keeps 1200 ± 100 DEG C, 4~6h again afterwards, imports the mixed gas of propane and argon gas, and propane and argon gas mixed proportion are 1:3, Mixture pressure is 0.2~0.4Mpa, and the flow velocity of mixed gas is 2~3m3/h。
The purpose designed in this way is, carries out surface coated treatment by gas-phase deposition, is finished having finished Polished part be placed in gaseous phase deposition stove, so that polished part surface is formed functional metal, nonmetallic by gas-phase deposition Or compound coat, high temperature salpeter solution directly etching carbon carbon crucible is avoided by face coat, improves the corrosion resistant of carbon carbon crucible Erosion ability.
Beneficial effects of the present invention include at least following one；
1, woven fabric is carried out using T700 12K carbon fibers and T700 6K carbon fibers, the mechanical strength of integral material can be improved, prevented It is only cracked in following process or the phenomenon that burst.
2, the processing scheme being combined using CVI and CVD, CVI, that is, Chemical Vapor Infiltration chemistry Gas-phase permeation can penetrate into reactant gas inside precast body, occur to chemically react and deposited, prefabricated component is made to be molded. Using CVD, that is, chemical vapor deposition chemical vapor depositions, entire work piece surface is carried out at coating Reason is allowed to after the size for increasing carbon carbon crucible, and entire crucible internal performance and external performance can meet needs, is solved existing In the preparation for having carbon carbon crucible, there are difficulty, reliability reduces, it is more difficult to be suitable for 26 inch or more for the molding of large scale graphite product The problem of carbon carbon crucible is processed.
3, its mechanical strength can be greatly improved, is made without the intertexture through weft yarn by using the interleaving mode of plain weave It is even closer to obtain entire yarn arrangement.
4, surface coated treatment is carried out by gas-phase deposition, the polished part finished will have been finished is placed in gas phase and has sunk In product stove, so that polished part surface is formed functional metal, nonmetallic or compound coat by gas-phase deposition, pass through table Finishing coat avoids high temperature salpeter solution directly etching carbon carbon crucible, improves the corrosion resistance of carbon carbon crucible.
Specific implementation mode
It is clear in order to enable the objectives, technical solutions, and advantages of the present invention to be more clear, with reference to embodiments to this Invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, not For limiting present invention protection content.
Embodiment 1
A kind of method that carbon fiber prepares large-size carbon carbon crucible, includes the following steps：
The first step, woven fabric select T700 12K carbon fibers and T700 6K carbon fibers, two kinds of carbon fibers are interleaved, are prepared into Prefabricated component；
Prefabricated component is completed infiltration molding by CVI densifications, is prepared into molded part by second step, material molding；
Third walks, and molded part is placed into heating furnace by high-temperature heat treatment, vacuumizes heating, surface of shaped parts pressure for- Argon gas is passed through after 0.08mpa to normal pressure, molded part is taken out in blow-on；
Molded part is prepared into the single piece of crucible shape by mechanical processing, then single piece is led to by the 4th step, processing, polishing It crosses polishing machine to be polished outer surface, is prepared into polished part；
Polished part is placed into gaseous phase deposition stove by the 5th step, surface coated treatment, vacuumizes heating, after reaching temperature, is passed through Propane and argon gas are deposited, and continue to vacuumize after deposition, are stood, blow-on, and carbon carbon crucible is taken out.
In use, carrying out woven fabric using T700 12K carbon fibers and T700 6K carbon fibers, the machine of integral material can be improved Tool intensity prevents cracked in following process or the phenomenon that burst.The processing scheme being combined using CVI and CVD, CVI That is Chemical Vapor Infiltration chemical vapor infiltrations, can penetrate into reactant gas inside precast body, hair Biochemical reaction is simultaneously deposited, and prefabricated component is made to be molded.Using CVD, that is, chemical vapor deposition chemistry gas It mutually deposits, coating treatment is carried out to entire work piece surface, is allowed to after the size for increasing carbon carbon crucible, property inside entire crucible It can meet needs with external performance, in the preparation for solving existing carbon carbon crucible, the molding of large scale graphite product exists Difficulty, reliability reduce, it is more difficult to be suitable for the problem of above carbon carbon crucible of 26 inch is processed.
Embodiment 2
A kind of method that carbon fiber prepares large-size carbon carbon crucible, includes the following steps：
The first step, woven fabric select T700 12K carbon fibers and T700 6K carbon fibers, by T700 12K carbon fibers and T700 6K carbon Fiber is interleaved as basic material, and the texture that interweaves is plain weave, is prepared into prefabricated component；
Prefabricated component is completed infiltration molding by CVI densifications, is prepared into molded part by second step, material molding；
Third walks, and molded part is placed into heating furnace by high-temperature heat treatment, vacuumizes heating, surface of shaped parts pressure for- Argon gas is passed through after 0.08mpa to normal pressure, molded part is taken out in blow-on；
Molded part is prepared into the single piece of crucible shape by mechanical processing, then single piece is led to by the 4th step, processing, polishing It crosses polishing machine to be polished outer surface, is prepared into polished part；
Polished part is placed into gaseous phase deposition stove by the 5th step, surface coated treatment, vacuumizes heating, after reaching temperature, is passed through Propane and argon gas are deposited, and continue to vacuumize after deposition, are stood, blow-on, and carbon carbon crucible is taken out.
In use, carrying out woven fabric using T700 12K carbon fibers and T700 6K carbon fibers, the machine of integral material can be improved Tool intensity prevents cracked in following process or the phenomenon that burst.The processing scheme being combined using CVI and CVD, CVI That is Chemical Vapor Infiltration chemical vapor infiltrations, can penetrate into reactant gas inside precast body, hair Biochemical reaction is simultaneously deposited, and prefabricated component is made to be molded.Using CVD, that is, chemical vapor deposition chemistry gas It mutually deposits, coating treatment is carried out to entire work piece surface, is allowed to after the size for increasing carbon carbon crucible, property inside entire crucible It can meet needs with external performance, in the preparation for solving existing carbon carbon crucible, the molding of large scale graphite product exists Difficulty, reliability reduce, it is more difficult to be suitable for the problem of above carbon carbon crucible of 26 inch is processed.Using the interleaving mode of plain weave, without The intertexture through weft yarn is crossed, its mechanical strength can be greatly improved so that entire yarn arrangement is even closer.
Embodiment 3
A kind of method that carbon fiber prepares large-size carbon carbon crucible, includes the following steps：
The first step, woven fabric select T700 12K carbon fibers and T700 6K carbon fibers, by T700 12K carbon fibers and T700 6K carbon Fiber is interleaved as basic material, and the texture that interweaves is plain weave, is prepared into prefabricated component；
Prefabricated component is placed into gas-phase permeation stove, vacuumizes, keeps pressure, then rise by second step, material molding, material molding Temperature keeps temperature in CVI infiltration stoves, is passed through propane gas, is permeated, and material molding vacuumizes pressure in rear gas-phase permeation stove For 4KPa, holding pressure time is 0.5h, and heating parameter is that temperature in the gas-phase permeation stove in vacuum is first promoted to 800 DEG C, and 0.5h is kept, then temperature in the gas-phase permeation stove in vacuum is promoted to 1300 DEG C from 800 DEG C, propane is passed through after 6h Gas makes pressure in gas-phase permeation stove fall to 1KPa, keeps 80h, be prepared into molded part；
Third walks, and molded part is placed into heating furnace by high-temperature heat treatment, vacuumizes heating, surface of shaped parts pressure for- Argon gas is passed through after 0.08mpa to normal pressure, molded part is taken out in blow-on；
Molded part is prepared into the single piece of crucible shape by mechanical processing, then single piece is led to by the 4th step, processing, polishing It crosses polishing machine to be polished outer surface, is prepared into polished part；
Polished part is placed into gaseous phase deposition stove by the 5th step, surface coated treatment, vacuumizes heating, after reaching temperature, is passed through Propane and argon gas are deposited, and continue to vacuumize after deposition, are stood, blow-on, and carbon carbon crucible is taken out.
In use, carrying out woven fabric using T700 12K carbon fibers and T700 6K carbon fibers, the machine of integral material can be improved Tool intensity prevents cracked in following process or the phenomenon that burst.The processing scheme being combined using CVI and CVD, CVI That is Chemical Vapor Infiltration chemical vapor infiltrations, can penetrate into reactant gas inside precast body, hair Biochemical reaction is simultaneously deposited, and prefabricated component is made to be molded.Using CVD, that is, chemical vapor deposition chemistry gas It mutually deposits, coating treatment is carried out to entire work piece surface, is allowed to after the size for increasing carbon carbon crucible, property inside entire crucible It can meet needs with external performance, in the preparation for solving existing carbon carbon crucible, the molding of large scale graphite product exists Difficulty, reliability reduce, it is more difficult to be suitable for the problem of above carbon carbon crucible of 26 inch is processed.Using the interleaving mode of plain weave, without The intertexture through weft yarn is crossed, its mechanical strength can be greatly improved so that entire yarn arrangement is even closer.Gas-phase permeation stove is taken out More gradient-heateds are carried out after vacuum, the applied stress being allowed between carbon carbon fiber can be released, and improve the durable of integral material Performance.
Embodiment 4
A kind of method that carbon fiber prepares large-size carbon carbon crucible, includes the following steps：
The first step, woven fabric select T700 12K carbon fibers and T700 6K carbon fibers, by T700 12K carbon fibers and T700 6K carbon Fiber is interleaved as basic material, and the texture that interweaves is plain weave, is prepared into prefabricated component；
Prefabricated component is placed into gas-phase permeation stove, vacuumizes, keeps pressure, then rise by second step, material molding, material molding Temperature keeps temperature in CVI infiltration stoves, is passed through propane gas, is permeated, and material molding vacuumizes pressure in rear gas-phase permeation stove For 10KPa, holding pressure time is 1h, and heating parameter is that temperature in the gas-phase permeation stove in vacuum is first promoted to 800 DEG C, and 0.5h is kept, then temperature in the gas-phase permeation stove in vacuum is promoted to 1300 DEG C from 800 DEG C, propane is passed through after 8h Gas makes pressure in gas-phase permeation stove fall to 2KPa, keeps 80h, be prepared into molded part；
Third walks, and molded part is placed into heating furnace by high-temperature heat treatment, vacuumizes heating, surface of shaped parts pressure for- Argon gas is passed through after 0.08mpa to normal pressure, molded part is taken out in blow-on, and wherein heating parameters are to promote furnace temp from room temperature To 1000 DEG C, temperature increase rate is 300 DEG C/h, furnace temp is then promoted to 2000 DEG C from 1000 DEG C, temperature is promoted Rate is 150 DEG C/h, then furnace temp is promoted to 2500 DEG C from 2000 DEG C, and temperature increase rate is 70 DEG C/h, is finally added Hot stove temperature is maintained at 2500 DEG C, 5h；
Molded part is prepared into the single piece of crucible shape by mechanical processing, then single piece is led to by the 4th step, processing, polishing It crosses polishing machine to be polished outer surface, is prepared into polished part, wherein polishing degree is 0.1 μm of Ra <；
Polished part is placed into gaseous phase deposition stove by the 5th step, surface coated treatment, vacuumizes heating, after reaching temperature, is passed through Propane and argon gas are deposited, and continue to vacuumize after deposition, are stood, blow-on, and carbon carbon crucible is taken out.
In use, carrying out woven fabric using T700 12K carbon fibers and T700 6K carbon fibers, the machine of integral material can be improved Tool intensity prevents cracked in following process or the phenomenon that burst.The processing scheme being combined using CVI and CVD, CVI That is Chemical Vapor Infiltration chemical vapor infiltrations, can penetrate into reactant gas inside precast body, hair Biochemical reaction is simultaneously deposited, and prefabricated component is made to be molded.Using CVD, that is, chemical vapor deposition chemistry gas It mutually deposits, coating treatment is carried out to entire work piece surface, is allowed to after the size for increasing carbon carbon crucible, property inside entire crucible It can meet needs with external performance, in the preparation for solving existing carbon carbon crucible, the molding of large scale graphite product exists Difficulty, reliability reduce, it is more difficult to be suitable for the problem of above carbon carbon crucible of 26 inch is processed.Using the interleaving mode of plain weave, without The intertexture through weft yarn is crossed, its mechanical strength can be greatly improved so that entire yarn arrangement is even closer.Gas-phase permeation stove is taken out More gradient-heateds are carried out after vacuum, the applied stress being allowed between carbon carbon fiber can be released, and improve the durable of integral material Performance.When carrying out high-temperature process, more gradient-heateds are carried out, the applied stress being allowed between carbon carbon fiber can be released, and be improved The durable performance of integral material.
Embodiment 5
A kind of method that carbon fiber prepares large-size carbon carbon crucible, includes the following steps：
The first step, woven fabric select T700 12K carbon fibers and T700 6K carbon fibers, by T700 12K carbon fibers and T700 6K carbon Fiber is interleaved as basic material, and the texture that interweaves is plain weave, is prepared into prefabricated component；
Prefabricated component is placed into gas-phase permeation stove, vacuumizes, keeps pressure, then rise by second step, material molding, material molding Temperature keeps temperature in CVI infiltration stoves, is passed through propane gas, is permeated, and material molding vacuumizes pressure in rear gas-phase permeation stove For 10KPa, holding pressure time is 1h, and heating parameter is that temperature in the gas-phase permeation stove in vacuum is first promoted to 800 DEG C, and 0.5h is kept, then temperature in the gas-phase permeation stove in vacuum is promoted to 1300 DEG C from 800 DEG C, propane is passed through after 8h Gas makes pressure in gas-phase permeation stove fall to 2KPa, keeps 80h, be prepared into molded part；
Third walks, and molded part is placed into heating furnace by high-temperature heat treatment, vacuumizes heating, surface of shaped parts pressure for- Argon gas is passed through after 0.08mpa to normal pressure, molded part is taken out in blow-on, and wherein heating parameters are to promote furnace temp from room temperature To 1000 DEG C, temperature increase rate is 100 DEG C/h, furnace temp is then promoted to 2000 DEG C from 1000 DEG C, temperature is promoted Rate is 50 DEG C/h, then furnace temp is promoted to 2500 DEG C from 2000 DEG C, and temperature increase rate is 30 DEG C/h, finally heated Furnace temperature is maintained at 2500 DEG C, 3h；
Molded part is prepared into the single piece of crucible shape by mechanical processing, then single piece is led to by the 4th step, processing, polishing It crosses polishing machine to be polished outer surface, is prepared into polished part, wherein polishing degree is 0.1 μm of Ra <；
Polished part is placed into gaseous phase deposition stove by the 5th step, surface coated treatment, vacuumizes heating, after reaching temperature, is passed through Propane and argon gas are deposited, and continue to vacuumize after deposition, are stood, blow-on, carbon carbon crucible are taken out, wherein polished part is put After being placed in gaseous phase deposition stove evacuation, gaseous phase deposition furnace pressure is 4KPa, and heating parameters are, by gaseous phase deposition in-furnace temperature from Room temperature is promoted to 1300 DEG C, then keeps 1100 DEG C, 6h again, imports the mixed gas of propane and argon gas, and propane and argon gas are mixed Composition and division in a proportion example is 1:The flow velocity of 3, mixture pressure 0.2Mpa, mixed gas are 3m3/h。
In use, carrying out woven fabric using T700 12K carbon fibers and T700 6K carbon fibers, the machine of integral material can be improved Tool intensity prevents cracked in following process or the phenomenon that burst.The processing scheme being combined using CVI and CVD, CVI That is Chemical Vapor Infiltration chemical vapor infiltrations, can penetrate into reactant gas inside precast body, hair Biochemical reaction is simultaneously deposited, and prefabricated component is made to be molded.Using CVD, that is, chemical vapor deposition chemistry gas It mutually deposits, coating treatment is carried out to entire work piece surface, is allowed to after the size for increasing carbon carbon crucible, property inside entire crucible It can meet needs with external performance, in the preparation for solving existing carbon carbon crucible, the molding of large scale graphite product exists Difficulty, reliability reduce, it is more difficult to be suitable for the problem of above carbon carbon crucible of 26 inch is processed.Using the interleaving mode of plain weave, without The intertexture through weft yarn is crossed, its mechanical strength can be greatly improved so that entire yarn arrangement is even closer.Gas-phase permeation stove is taken out More gradient-heateds are carried out after vacuum, the applied stress being allowed between carbon carbon fiber can be released, and improve the durable of integral material Performance.When carrying out high-temperature process, more gradient-heateds are carried out, the applied stress being allowed between carbon carbon fiber can be released, and be improved The durable performance of integral material.Surface coated treatment is carried out by gas-phase deposition, the polished part finished will have been finished It is placed in gaseous phase deposition stove, so that polished part surface is formed functional metal, nonmetallic or compound by gas-phase deposition Coating avoids high temperature salpeter solution directly etching carbon carbon crucible by face coat, improves the corrosion resistance of carbon carbon crucible.

Claims (7)

1. a kind of method that carbon fiber prepares large-size carbon carbon crucible, it is characterised in that：Include the following steps：
The first step, woven fabric select T700 12K carbon fibers and T700 6K carbon fibers, two kinds of carbon fibers are interleaved, are prepared into Prefabricated component；
Prefabricated component is completed infiltration molding by CVI densifications, is prepared into molded part by second step, material molding；
Third walks, and molded part is placed into heating furnace by high-temperature heat treatment, vacuumizes heating, surface of shaped parts pressure for- Argon gas is passed through after 0.08mpa to normal pressure, molded part is taken out in blow-on；
Molded part is prepared into the single piece of crucible shape by mechanical processing, then single piece is led to by the 4th step, processing, polishing It crosses polishing machine to be polished outer surface, is prepared into polished part；
Polished part is placed into gaseous phase deposition stove by the 5th step, surface coated treatment, vacuumizes heating, after reaching temperature, is passed through Propane and argon gas are deposited, and continue to vacuumize after deposition, are stood, blow-on, and carbon carbon crucible is taken out.
2. the method that a kind of carbon fiber according to claim 1 prepares large-size carbon carbon crucible, it is characterised in that：Described T700 12K carbon fibers are interleaved with T700 6K carbon fibers as basic material by one step, woven fabric, and the texture that interweaves For plain weave.
3. the method that a kind of carbon fiber according to claim 2 prepares large-size carbon carbon crucible, it is characterised in that：Described Two steps, material molding, prefabricated component is placed into gas-phase permeation stove, is vacuumized, and keeps pressure, then is heated up and kept CVI infiltration stoves Middle temperature, is passed through propane gas, is permeated.
4. the method that a kind of carbon fiber according to claim 3 prepares large-size carbon carbon crucible, it is characterised in that：Described Two steps, material molding, it is 4~10KPa to vacuumize pressure in rear gas-phase permeation stove, and holding pressure time is 0.5~1h, heating ginseng Number is temperature in the gas-phase permeation stove in vacuum to be first promoted to 800 DEG C, and keep 0.5h, then by the gas phase in vacuum Temperature is promoted to 1300 DEG C from 800 DEG C in infiltration stove, and propane gas is passed through after 6~8h, pressure in gas-phase permeation stove is made to fall to 1 ~2KPa keeps 80h.
5. the method that a kind of carbon fiber according to claim 4 prepares large-size carbon carbon crucible, it is characterised in that：Described Three steps, high-temperature heat treatment, heating parameters are furnace temp to be promoted to 1000 DEG C from room temperature, temperature increase rate 100 DEG C/h~300 DEG C/h, furnace temp is then promoted to 2000 DEG C from 1000 DEG C, temperature increase rate is 50 DEG C/h~150 DEG C/h, then furnace temp is promoted to 2500 DEG C from 2000 DEG C, temperature increase rate is 30 DEG C/h~70 DEG C/h, finally heated Furnace temperature is maintained at 2500 DEG C, 3~5h.
6. the method that a kind of carbon fiber according to claim 5 prepares large-size carbon carbon crucible, it is characterised in that：Described Four steps, processing, polishing, polishing degree are 0.1 μm of Ra <.
7. the method that a kind of carbon fiber according to claim 6 prepares large-size carbon carbon crucible, it is characterised in that：Described Five steps, surface coated treatment, after polished part is placed into gaseous phase deposition stove evacuation, gaseous phase deposition furnace pressure be 4~ 10KPa, heating parameters are that gaseous phase deposition in-furnace temperature is promoted to 1200 ± 100 DEG C from room temperature, then keep 1200 again ± 100 DEG C, 4~6h, the mixed gas of propane and argon gas is imported, and propane and argon gas mixed proportion are 1:3, mixture pressure is The flow velocity of 0.2~0.4Mpa, mixed gas are 2~3m3/h。
CN201810600329.XA 2018-06-12 2018-06-12 A kind of method that carbon fiber prepares large-size carbon carbon crucible Pending CN108752031A (en)

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CN114920574A (en) * 2022-06-07 2022-08-19 醴陵市东方电瓷电器有限公司 Method for preparing large-size carbon-carbon crucible by three-dimensional weaving of carbon fibers

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