CN113277867A - Preparation method of carbon/silicon carbide composite material crucible - Google Patents
Preparation method of carbon/silicon carbide composite material crucible Download PDFInfo
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- CN113277867A CN113277867A CN202110509674.4A CN202110509674A CN113277867A CN 113277867 A CN113277867 A CN 113277867A CN 202110509674 A CN202110509674 A CN 202110509674A CN 113277867 A CN113277867 A CN 113277867A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 48
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 47
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 46
- 239000002131 composite material Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 64
- 239000004917 carbon fiber Substances 0.000 claims abstract description 63
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 61
- 238000000034 method Methods 0.000 claims abstract description 50
- 238000009958 sewing Methods 0.000 claims abstract description 38
- 239000004744 fabric Substances 0.000 claims abstract description 26
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000011248 coating agent Substances 0.000 claims abstract description 13
- 238000000576 coating method Methods 0.000 claims abstract description 13
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 11
- 238000005475 siliconizing Methods 0.000 claims abstract description 11
- 239000007789 gas Substances 0.000 claims abstract description 9
- 238000000197 pyrolysis Methods 0.000 claims abstract description 9
- 229910052786 argon Inorganic materials 0.000 claims abstract description 7
- 238000004519 manufacturing process Methods 0.000 claims abstract description 7
- 238000000151 deposition Methods 0.000 claims abstract description 6
- 238000003754 machining Methods 0.000 claims abstract description 6
- 239000012159 carrier gas Substances 0.000 claims abstract description 4
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims abstract description 4
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims abstract description 4
- 238000005470 impregnation Methods 0.000 claims description 19
- 238000007789 sealing Methods 0.000 claims description 18
- 238000006243 chemical reaction Methods 0.000 claims description 13
- 238000005336 cracking Methods 0.000 claims description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 5
- 239000010703 silicon Substances 0.000 claims description 5
- 238000004804 winding Methods 0.000 claims description 4
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 230000008020 evaporation Effects 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 229920003257 polycarbosilane Polymers 0.000 claims description 3
- 230000001681 protective effect Effects 0.000 claims description 3
- 239000011856 silicon-based particle Substances 0.000 claims description 3
- 238000003892 spreading Methods 0.000 claims description 3
- 239000008096 xylene Substances 0.000 claims description 3
- 238000005498 polishing Methods 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 abstract description 5
- 238000007254 oxidation reaction Methods 0.000 abstract description 5
- 239000011148 porous material Substances 0.000 abstract description 5
- 230000003628 erosive effect Effects 0.000 abstract description 4
- 230000002035 prolonged effect Effects 0.000 abstract 1
- 239000000047 product Substances 0.000 description 20
- 239000000835 fiber Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 230000007547 defect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 230000002401 inhibitory effect Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000011157 advanced composite material Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001721 carbon Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 230000002829 reductive effect Effects 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
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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
- 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
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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
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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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
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/62222—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining ceramic coatings
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5053—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials non-oxide ceramics
- C04B41/5057—Carbides
- C04B41/5059—Silicon carbide
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
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Abstract
The invention relates to the technical field of crucible preparation, and discloses a preparation method of a carbon/silicon carbide composite material crucible, which comprises the following steps: A) sequentially and alternately superposing carbon fiber plain cloth and a carbon fiber net tire on the core mold, and when the preset thickness is reached, manufacturing a crucible preform by a needling sewing process; B) taking propylene as a carbon source gas and argon as a carrier gas, depositing and densifying the preform by adopting a chemical vapor deposition process, and then performing repeated dipping-pyrolysis operation to prepare a crucible blank with a predetermined density; C) machining the crucible blank to prepare a crucible product; D) and (4) carrying out gas phase siliconizing on the crucible product to form a compact silicon carbide coating, and preparing the finished crucible product. The method fully utilizes the advantage of filling the inner pores of the prefabricated part by each process, and the compact silicon carbide coating is formed on the surface of the crucible product, so that the oxidation erosion can be effectively inhibited, and the service life of the crucible is greatly prolonged.
Description
Technical Field
The invention relates to the technical field of crucible preparation, in particular to a preparation method of a carbon/silicon carbide composite material crucible.
Background
The carbon/carbon composite material is one of the advanced composite materials widely used at present, is a composite material formed by carbon fibers or various carbon fabric reinforced carbon matrixes, and has the excellent performances of low density, high specific strength, wear resistance, high temperature resistance, small thermal expansion coefficient and the like. The material becomes one of important basic materials in the fields of aerospace, metallurgy, new energy and the like, and is an ideal substitute for graphite products and heat-resistant steel.
The tool in the single crystal furnace generally adopts a graphite crucible, the graphite crucible has poor mechanical property in a high-temperature environment, the service life is short, and the production cost of an enterprise is greatly increased. At present, part of the merchants adopt carbon/carbon composite materials to manufacture crucibles, but SiO is used in the process2The oxidation erosion can be carried out on the surface of the carbon/carbon composite material, and then the carbon/carbon composite material permeates into the crucible, so that the erosion in the crucible is aggravated, and the service life of the crucible is greatly influenced.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: provides a preparation method of a carbon/silicon carbide composite material crucible capable of forming a compact coating on the surface.
In order to solve the technical problem, the invention provides a preparation method of a carbon/silicon carbide composite material crucible, which comprises the following steps:
A) selecting a matched core mould according to the shape and structure of the crucible to be prepared, sequentially and alternately superposing carbon fiber plain cloth and a carbon fiber net blank on the core mould, and preparing a crucible preform by a needling sewing process when the predetermined thickness is reached;
B) taking propylene as a carbon source gas and argon as a carrier gas, depositing and densifying the prefabricated body by adopting a chemical vapor deposition process, and then performing repeated dipping-pyrolysis operation to prepare a crucible blank with a predetermined density;
C) according to the size of the crucible to be prepared, machining the crucible blank to prepare a crucible product;
D) and carrying out gas-phase siliconizing on the crucible product to form a compact silicon carbide coating on the surface of the crucible product, and preparing the finished product of the carbon/silicon carbide composite material crucible.
Preferably, the step a) is specifically:
according to the shape and structure of the crucible to be prepared, selecting a matched core mould, laying the carbon fiber plain cloth and the carbon fiber net tire on the core mould in sequence to serve as laying units, winding carbon fiber yarns on the outer side of each layer of the laying units in a crossed mode along the inclined direction, overlapping the laying units to a preset thickness layer by layer according to a fixed shape and outline, and manufacturing the crucible preform through a needling sewing process in the thickness direction.
Preferably, in the step a):
the carbon fiber plain cloth and the carbon fiber net tire are laid on the circular wall surface of the core mold to serve as a circular pipe section, the carbon fiber plain cloth and the carbon fiber net tire are laid on the circular bottom surface of the core mold to serve as a circular ring connecting section, the carbon fiber plain cloth and the carbon fiber net tire are laid on the flat bottom surface of the core mold to serve as a circular bottom sealing section, and the circular pipe section, the circular ring connecting section and the circular bottom sealing section are sequentially connected to form the layer spreading unit.
Preferably, in the step a):
and performing wave track sewing at the joint between the circular pipe section and the circular ring connecting section and the joint between the circular ring connecting section and the circular bottom sealing section.
Preferably, in the step a):
and sewing is carried out on the circular pipe section along the axial direction, and sewing is carried out on the circular ring connecting section along the annular direction.
Preferably, in the step a):
the needling sewing process adopts a single-side double-needle sewing process.
Preferably, in the step B):
the furnace pressure of the chemical vapor deposition is 1.5KPa to 2KPa, and the reaction temperature is 950 ℃ to 1000 ℃.
Preferably, in the step B):
mixing polycarbosilane and xylene into an impregnating solution, adding the impregnating solution into an impregnation cracking furnace, placing the densified preform into the impregnating solution for impregnation, wherein the impregnation time is 1-2 hours under a vacuum condition, discharging the impregnating solution after the impregnation is finished, introducing argon as a protective gas for high-temperature cracking at the cracking temperature of 1200-1300 ℃, and obtaining the density of 1.7g/cm3-1.8g/cm3The crucible blank of (1).
Preferably, in the step C):
and (3) polishing the crucible blank inside and outside according to the size of the crucible to be prepared to prepare a crucible product.
Preferably, in the step D):
and (3) placing the crucible product in a siliconizing furnace, heating silicon particles to an evaporation state, and infiltrating gaseous silicon into the surface of the crucible product to form a compact silicon carbide coating under the vacuum condition and at the reaction temperature of 1600-1700 ℃ to prepare the finished product of the carbon/silicon carbide composite material crucible.
Compared with the prior art, the preparation method of the carbon/silicon carbide composite material crucible provided by the invention has the beneficial effects that:
according to the invention, carbon fiber plain cloth and carbon fiber net tires are sequentially and alternately stacked on a core mold to form a specific crucible shape, and when the specific crucible shape is reached to a preset thickness, a crucible preform is manufactured through a needling sewing process. And then, a chemical vapor deposition process is adopted for rapid deposition densification, and repeated impregnation-pyrolysis operation is carried out, so that impregnation liquid can better penetrate through the interior of the fiber bundle of the prefabricated body and fill the pores among the corresponding fiber bundles, the compactness is further improved, the mechanical property is greatly improved, and the advantage that each process fills the pores in the prefabricated body is fully utilized. And finally, forming a compact silicon carbide coating on the surface of the crucible product in a gas-phase siliconizing mode, effectively inhibiting oxidation corrosion and greatly prolonging the service life of the crucible.
Drawings
FIG. 1 is a block flow diagram of a method of making a carbon/silicon carbide composite crucible according to a preferred embodiment of the present invention.
Fig. 2 is a schematic sectional structure view of a carbon/silicon carbide composite crucible preform according to a preferred embodiment of the present invention.
Fig. 3 is an enlarged view of a structure a in fig. 1.
Fig. 4 is an enlarged view of the structure at B in fig. 1.
FIG. 5 is a schematic view showing the structure of carbon fiber plain cloth and carbon fiber mesh in a carbon/silicon carbide composite crucible preform according to a preferred embodiment of the present invention.
Fig. 6 is a schematic view of the structure of carbon fiber filaments in a carbon/silicon carbide composite crucible preform according to a preferred embodiment of the present invention.
FIG. 7 is a schematic view of the stitched side view configuration of a carbon/silicon carbide composite crucible preform of the preferred embodiment of the present invention.
FIG. 8 is a schematic view of the stitched bottom structure of a carbon/silicon carbide composite crucible preform according to a preferred embodiment of the present invention.
In the figure: 1. carbon fiber plain cloth; 2. a carbon fiber mesh tire; 3. carbon fiber filaments; 4. a circular pipe section; 5. a circular ring connecting section; 6. a circular bottom sealing section.
Detailed Description
The invention is further described below with reference to the drawings and specific preferred embodiments of the description, without thereby limiting the scope of protection of the invention.
As shown in fig. 1, an embodiment of the present invention provides a method for preparing a carbon/silicon carbide composite crucible, including the following steps: the method comprises the following steps:
A) selecting a matched core mould according to the shape and structure of the crucible to be prepared, alternately stacking the carbon fiber plain cloth 1 and the carbon fiber net blank 2 on the core mould in sequence, and preparing a crucible preform by a needling sewing process when the thickness reaches a preset thickness;
B) taking propylene as a carbon source gas and argon as a carrier gas, depositing and densifying the prefabricated body by adopting a chemical vapor deposition process, and then performing repeated dipping-pyrolysis operation to prepare a crucible blank with a predetermined density;
C) according to the size of the crucible to be prepared, machining the crucible blank to prepare a crucible product;
D) and carrying out gas-phase siliconizing on the crucible product to form a compact silicon carbide coating on the surface of the crucible product, and preparing the finished product of the carbon/silicon carbide composite material crucible.
According to the preparation method of the carbon/silicon carbide composite material crucible, the carbon fiber plain cloth 1 and the carbon fiber net tire 2 are sequentially and alternately superposed on the core mold to form a specific crucible shape, and when the predetermined thickness is reached, the crucible preform is prepared through a needling sewing process. And then, a chemical vapor deposition process is adopted for rapid deposition densification, and repeated impregnation-pyrolysis operation is carried out, so that impregnation liquid can better penetrate through the interior of the fiber bundle of the prefabricated body and fill the pores among the corresponding fiber bundles, the compactness is further improved, the mechanical property is greatly improved, and the advantage that each process fills the pores in the prefabricated body is fully utilized. And finally, forming a compact silicon carbide coating on the surface of the crucible product in a gas-phase siliconizing mode, effectively inhibiting oxidation corrosion and greatly prolonging the service life of the crucible.
In this embodiment, the step a) specifically includes: according to the shape and structure of the crucible to be prepared, selecting a matched core mould, laying the carbon fiber plain cloth 1 and the carbon fiber net tire 2 on the core mould in sequence to serve as laying units, winding carbon fiber yarns 3 on the outer side of each layer of the laying units in a crossed mode along the inclined direction, overlapping the laying units to a preset thickness layer by layer according to a fixed shape profile, and manufacturing a crucible preform through a needling sewing process in the thickness direction. This mode can let and spread the layer unit core mould of laminating more, realizes better design effect, and follow-up machining need not to polish away too much material, and machining efficiency is high.
In this embodiment, the step a) further includes: the carbon fiber plain cloth 1 and the carbon fiber net tire 2 are laid on the circular wall surface of the core mold to serve as a circular pipe section 4, the carbon fiber plain cloth 1 and the carbon fiber net tire 2 are laid on the circular bottom surface of the core mold to serve as a circular ring connecting section 5, the carbon fiber plain cloth 1 and the carbon fiber net tire 2 are laid on the flat bottom surface of the core mold to serve as a circular bottom sealing section 6, and the circular pipe section 4, the circular ring connecting section 5 and the circular bottom sealing section 6 are sequentially connected to form the laying unit. As shown in fig. 2 to 4, the outer side edge of the circular ring connecting section 5 is connected to the circular opening at the bottom of the circular pipe section 4, and the inner side edge of the circular ring connecting section 5 is connected to the outer side edge of the circular bottom sealing section 6, so that the circular pipe section 4, the circular ring connecting section 5 and the circular bottom sealing section 6 form a cylindrical structure. As shown in fig. 5, the whole laying process is formed by stacking and laying, and the carbon fiber plain cloth 1 and the carbon fiber net tire 2 do not need to be stretched or compressed too much, so that the thickness of the formed prefabricated body is more uniform. Referring to fig. 6, the winding direction of the carbon fiber yarn 3 is 45 degrees or-45 degrees with the axial direction, and the carbon fiber yarn 3 wraps the circular tube section 4, the circular ring connecting section 5 and the circular bottom sealing section 6 to form an integral structure.
Further, in the step a): and (3) performing wave track sewing at the joint between the circular pipe section 4 and the circular ring connecting section 5 and the joint between the circular ring connecting section 5 and the circular bottom sealing section 6. As shown in fig. 7 to 8, the circumferential seams at the joints are sewn in a specific manner, so that the circumferential seams are tightly attached to each other, and the mechanical property defect at the joints is avoided. Wherein, the direction of each section of sewing thread changes the sewing direction by swinging the prefabricated body in the sewing process, thereby forming a wavy sewing track.
Further, in the step a): the circular pipe section 4 is sewn along the axial direction, sewing is facilitated, and the distance between every two adjacent sewing tracks is adjusted according to actual conditions. The carbon fiber plain cloth 1 and the carbon fiber net tire 2 on the circular pipe section 4 are in strip shapes, the carbon fiber plain cloth 1 and the carbon fiber net tire 2 in the strip shapes are coated on the circular wall surface of the core mold to form the circular pipe section 4, seams of the carbon fiber plain cloth 1 on the circular pipe section 4 are staggered with seams of the carbon fiber net tire 2, and mechanical property defects caused by overlapping of the seams can be avoided.
Further, in the step a): the circular ring connecting section 5 is sewed along the annular direction, sewing is convenient, and the distance between two adjacent sewing tracks is adjusted according to actual conditions. It is understood that if the circular bottom section 6 has a larger area, the circular bottom section 6 is also sewn, and the sewing path is in a ring shape. The carbon fiber plain cloth 1 and the carbon fiber net tire 2 on the circular ring connecting section 5 are circular rings, so that the circular ring connecting section 5 cannot form a seam, and the mechanical property of the circular ring connecting section is guaranteed. Similarly, the carbon fiber plain cloth 1 and the carbon fiber net tire 2 on the circular bottom sealing section 6 are circular, so that a seam cannot be formed on the circular bottom sealing section 6, and the mechanical property of the circular bottom sealing section is ensured.
In this embodiment, in the step a): the needling sewing process adopts a single-side double-needle sewing process, namely, in the sewing process, both a thread guiding needle and a thread hooking needle of the needling sewing process are manually/automatically sewn on the outer side of the prefabricated body, the needling sewing process is not influenced by the shape and the structure, the continuous and stable sewing is ensured, and the material performance is also enhanced.
In this embodiment, in step B): the furnace pressure of the chemical vapor deposition is 1.5KPa-2KPa (preferably 2KPa), the reaction temperature is 950 ℃ -1000 ℃ (preferably 960 ℃), and the density of the obtained crucible blank is 1.5g/cm3。
In this embodiment, in step B): mixing polycarbosilane and xylene (in a ratio of 10:1) to form an impregnation solution, adding the impregnation solution into an impregnation cracking furnace, placing the densified preform into the impregnation solution for impregnation, wherein the impregnation time is 1-2 hours (preferably 2 hours) under a vacuum condition, and then introducing air for impregnation for 10 hours. After the impregnation is finished, discharging the impregnation liquid, introducing argon as protective gas to carry out pyrolysis at 1200-1300 ℃ (1200 ℃ is preferred), repeating for 6 times at 1 hour to obtain the density of 1.7g/cm3-1.8g/cm3The crucible blank of (1).
In this embodiment, in step C): and according to the size of the crucible to be prepared, the crucible blank is polished inside and outside, the forming effect is good, and excessive materials do not need to be polished off to prepare a crucible product.
In this embodiment, in step D): placing the crucible product in the siliconizing furnace, heating silicon particles to an evaporation state, infiltrating gaseous silicon into the surface of the crucible product to form a compact silicon carbide coating under the vacuum condition and at a reaction temperature of 1600-1700 ℃ (1650 ℃ is preferred), and preparing the finished product of the carbon/silicon carbide composite crucible, wherein the density of the finished product is 2.24g/cm3. Wherein, the reaction process is roughly divided into two stages: in the first stage, after contacting carbon fibers, gaseous silicon adsorbs the carbon fibers and undergoes a chemical reaction to form silicon carbide, and the surface of the fibers is wrapped to form a thin layer which is then reacted for the next stage; and in the second stage, the reaction is a diffusion reaction of carbon and silicon in the silicon carbide layer, and the reaction rate is slowed down until the reaction space is reduced continuously along with the increase of the thickness of the silicon carbide coating.
The steps of the chemical vapor deposition process, the dipping-pyrolysis process and the gas phase siliconizing reaction sintering process used in the above embodiments are all conventional steps, the unrecited process parameters are also conventional process parameters, the data of the density, the SiC content and the like of the sample are measured according to a conventional method, and the chemical vapor deposition furnace, the pyrolysis furnace, the siliconizing furnace and other equipment are all commercially available.
In summary, the embodiment of the present invention provides a method for preparing a carbon/silicon carbide composite crucible, which has the following advantages: (1) can form a compact silicon carbide coating on the surface, can effectively inhibit oxidation erosion and greatly prolong the service life of the crucible. (2) The layer spreading unit of the prefabricated body is formed by combining a circular pipe section 4, a circular ring connecting section 5 and a circular bottom sealing section 6, and the outer side of the prefabricated body is crossed and wound by carbon fiber yarns 3 to be attached to a core mold, so that the shaping effect is good. (3) The needling sewing is a single-side double-needle sewing process, the sewing process is not influenced by the internal shape structure, and the circumferential seams between the circular pipe section 4 and the circular bottom sealing section 6 and the circular ring connecting section 5 are sewn by adopting wavy tracks, so that the mechanical property defect at the connecting part is avoided.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and substitutions can be made without departing from the technical principle of the present invention, and these modifications and substitutions should also be regarded as the protection scope of the present invention.
Claims (10)
1. A preparation method of a carbon/silicon carbide composite material crucible is characterized by comprising the following steps:
A) selecting a matched core mould according to the shape and structure of the crucible to be prepared, sequentially and alternately superposing carbon fiber plain cloth and a carbon fiber net blank on the core mould, and preparing a crucible preform by a needling sewing process when the predetermined thickness is reached;
B) taking propylene as a carbon source gas and argon as a carrier gas, depositing and densifying the prefabricated body by adopting a chemical vapor deposition process, and then performing repeated dipping-pyrolysis operation to prepare a crucible blank with a predetermined density;
C) according to the size of the crucible to be prepared, machining the crucible blank to prepare a crucible product;
D) and carrying out gas-phase siliconizing on the crucible product to form a compact silicon carbide coating on the surface of the crucible product, and preparing the finished product of the carbon/silicon carbide composite material crucible.
2. The method for preparing a carbon/silicon carbide composite crucible according to claim 1, wherein the step a) is specifically:
according to the shape and structure of the crucible to be prepared, selecting a matched core mould, laying the carbon fiber plain cloth and the carbon fiber net tire on the core mould in sequence to serve as laying units, winding carbon fiber yarns on the outer side of each layer of the laying units in a crossed mode along the inclined direction, overlapping the laying units to a preset thickness layer by layer according to a fixed shape and outline, and manufacturing the crucible preform through a needling sewing process in the thickness direction.
3. The method for preparing a carbon/silicon carbide composite crucible according to claim 2, wherein in the step a):
the carbon fiber plain cloth and the carbon fiber net tire are laid on the circular wall surface of the core mold to serve as a circular pipe section, the carbon fiber plain cloth and the carbon fiber net tire are laid on the circular bottom surface of the core mold to serve as a circular ring connecting section, the carbon fiber plain cloth and the carbon fiber net tire are laid on the flat bottom surface of the core mold to serve as a circular bottom sealing section, and the circular pipe section, the circular ring connecting section and the circular bottom sealing section are sequentially connected to form the layer spreading unit.
4. The method for preparing a carbon/silicon carbide composite crucible according to claim 3, wherein in the step A):
and performing wave track sewing at the joint between the circular pipe section and the circular ring connecting section and the joint between the circular ring connecting section and the circular bottom sealing section.
5. The method for preparing a carbon/silicon carbide composite crucible according to claim 3, wherein in the step A):
and sewing is carried out on the circular pipe section along the axial direction, and sewing is carried out on the circular ring connecting section along the annular direction.
6. The method for preparing a carbon/silicon carbide composite crucible according to claim 2, wherein in the step a):
the needling sewing process adopts a single-side double-needle sewing process.
7. The method for preparing a carbon/silicon carbide composite crucible according to claim 1, wherein in the step B):
the furnace pressure of the chemical vapor deposition is 1.5KPa to 2KPa, and the reaction temperature is 950 ℃ to 1000 ℃.
8. The method for preparing a carbon/silicon carbide composite crucible according to claim 7, wherein in the step B):
mixing polycarbosilane and xylene into an impregnating solution, adding the impregnating solution into an impregnation cracking furnace, placing the densified preform into the impregnating solution for impregnation, wherein the impregnation time is 1-2 hours under a vacuum condition, discharging the impregnating solution after the impregnation is finished, introducing argon as a protective gas for high-temperature cracking at the cracking temperature of 1200-1300 ℃, and obtaining the density of 1.7g/cm3-1.8g/cm3The crucible blank of (1).
9. The method for preparing a carbon/silicon carbide composite crucible according to claim 1, wherein in the step C):
and (3) polishing the crucible blank inside and outside according to the size of the crucible to be prepared to prepare a crucible product.
10. The method for preparing a carbon/silicon carbide composite crucible according to claim 1, wherein in the step D):
and (3) placing the crucible product in a siliconizing furnace, heating silicon particles to an evaporation state, and infiltrating gaseous silicon into the surface of the crucible product to form a compact silicon carbide coating under the vacuum condition and at the reaction temperature of 1600-1700 ℃ to prepare the finished product of the carbon/silicon carbide composite material crucible.
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