CN112876274B - Production process of carbon/carbon composite material crucible prefabricated part - Google Patents
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- C04B35/71—Ceramic products containing macroscopic reinforcing agents
- C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
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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
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- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
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Abstract
The invention discloses a production process of a carbon/carbon composite material crucible prefabricated part, and relates to the technical field of carbon material preparation. The method comprises the following steps: (1) respectively weaving a net tire and carbon cloth by using carbon fiber raw materials, weaving sandwich cloth by using nano fibers and carbon fibers in a mixed manner, arranging the sandwich between the net tire and the carbon cloth, compounding the sandwich into a felt through needling, and then overlapping and winding the needled carbon cloth and the net tire to obtain a carbon fiber woven part; (2) soaking the carbon fiber woven piece in a soaking solution, and performing ultrasonic auxiliary treatment, wherein the soaking solution comprises a solvent, nano particles and epoxy resin, the soaking temperature is 50-95 ℃, and the soaking time is 30-150 min; (3) and drying the impregnated carbon fiber woven piece to obtain the crucible prefabricated piece. The prefabricated part obtained by the invention can effectively improve the deposition speed of carbon atoms on a woven material during vapor deposition, realizes rapid densification, and has good mechanical property and long service life.
Description
Technical Field
The invention relates to the technical field of carbon material preparation, in particular to a production process of a carbon/carbon composite crucible prefabricated part.
Background
The carbon/carbon composite material is a novel high-performance structural function composite material which is formed by taking multidimensional braided carbon fibers as a reinforcing phase and taking pyrolytic carbon formed by chemical vapor infiltration or liquid phase impregnation cracking as a matrix, has the advantages of low density, high elastic modulus, large specific strength, low coefficient of thermal expansion, good corrosion resistance and high-temperature performance and the like, and has good application prospect in the fields of aerospace, chemical engineering, metallurgy, nuclear energy and the like.
In recent years, with the popularization and application of carbon/carbon composite materials in the aspect of civil equipment, many companies adopt carbon/carbon composite material crucibles to replace isostatic graphite crucibles, the carbon/carbon composite material crucibles are crucible preforms woven by taking carbon fibers as raw materials, and then matrix carbon reinforced fiber structures are obtained by adopting methods such as a chemical vapor deposition process, a chemical vapor infiltration process, an impregnation process and the like. However, in the conventional CVI method such as the isothermal CVI method, the deposition rate is generally between 2.78 and 6.94 multiplied by 10 to 5 mu m/s because the deposition process is controlled by diffusion and transmission of carbon source gases, so that the densification period of the carbon/carbon composite material is as long as hundreds of hours, the efficiency is low, the cost is high, and the popularization and application of the carbon/carbon composite material are seriously restricted.
Chinese patent application 201510909260.5 discloses a preparation method of a metal type C/C composite material carbon slide bar, belonging to the technical field of material preparation for electric locomotives. The single-layer 0-degree weftless carbon cloth, the carbon fiber net tire, the graphite powder, the copper material, the single-layer 90-degree weftless carbon cloth, the carbon fiber net tire, the graphite powder, the copper material and the single-layer 0-degree weftless carbon cloth are sequentially and circularly superposed, the relay needling method is adopted to introduce the carbon fiber bundles in the direction vertical to the layering direction to prepare a 2.5D carbon fiber needled integral felt with the density of 0.6-2.6g/cm3, and then the 2.5D carbon fiber needled integral felt is subjected to chemical vapor deposition pyrolytic carbon treatment; obtaining a C/C-Cu composite material; and finally, according to the size of the designed slide bar, carrying out mechanical processing on the obtained C/C-Cu composite material, reserving a processing allowance, and then carrying out polymer impregnation-carbonization treatment to obtain a finished product. The preparation process is simple, and the prepared metal type C/C composite material has lower resistivity and high heat capacity.
Chinese patent application 201210166266.4 discloses a preparation process of a carbon/carbon composite material crucible for a monocrystalline silicon furnace, which adopts a prefabricated body woven by polyacrylonitrile-based carbon fibers, takes mixed gas of natural gas, propylene and liquefied petroleum gas as a carbon source, takes nitrogen or argon as carrier gas, and forms uniform temperature heat in a vertical tank type deposition furnaceIn the field, the upper air inlet and the lower air inlet of the pipeline are switched at regular time, the combination of a temperature equalizing method, a pressure difference method and a forced airflow method is realized by utilizing the pressure difference of the air inside and outside the crucible, the integral rapid densification of the crucible woven piece is realized, and the density of the crucible can reach 1.6g/cm after 300 to 350 hours3Compared with the traditional free deposition process, the method greatly shortens the deposition time and reduces the production cost. After the crucible is mechanically processed, the crucible is used in a thermal field of a monocrystalline silicon furnace, the service life of the carbon/carbon composite material crucible is prolonged by 3 to 5 times compared with a hot isostatic pressing graphite crucible, the cost performance is obviously superior to that of the graphite crucible, and the production cost and labor intensity of monocrystalline silicon are greatly reduced. This method is still time consuming.
In view of the above, the present application provides a production process of a carbon/carbon composite crucible preform, which improves the deposition rate of carbon atoms on a woven material by improving the structure of the material, so as to realize rapid densification, and the prepared crucible preform has good mechanical properties and a prolonged service life.
Disclosure of Invention
The invention aims to provide a production process of a carbon/carbon composite crucible prefabricated part, which is characterized in that a nanometer material layer and nanometer particles are added into a material, and meanwhile, the vapor deposition process conditions are controlled, so that the deposition speed of carbon atoms on a woven part material can be effectively increased during vapor deposition of the woven part, the rapid densification is realized, the deposition time is shortened, and meanwhile, good mechanical properties and long service life are obtained.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a production process of a carbon/carbon composite material crucible prefabricated member comprises the following steps:
(1) preparing a carbon fiber woven piece: respectively weaving a net tire and carbon cloth by using carbon fiber raw materials, weaving sandwich cloth by using nano fibers and carbon fibers in a mixed manner, arranging a sandwich layer between the net tire and the carbon cloth, compounding the sandwich layer into a felt through needling, winding the felt on a crucible mold, and overlapping and winding the needled carbon cloth and the net tire until the density reaches 0.2-0.7g/cm3 to obtain a carbon fiber woven piece;
(2) dipping treatment: completely soaking the carbon fiber woven piece obtained in the step (1) in a soaking solution, and performing ultrasonic-assisted treatment, wherein the soaking solution comprises a solvent, nano particles and epoxy resin, the soaking temperature is 50-95 ℃, and the soaking time is 30-150 min;
(3) and drying the impregnated carbon fiber woven piece to obtain the carbon/carbon composite material crucible prefabricated piece.
Preferably, in the step (1), the mass ratio of the nanofibers to the carbon fibers in the sandwich cloth is 1:40-80, and more preferably 1: 50.
Preferably, in the step (1), the preparation method of the sandwich cloth comprises the following steps: weaving the carbon fiber into a cloth piece, soaking the cloth piece into the dispersed nanofiber solution, filtering to remove the solvent to enable the nanofiber to be left on the cloth piece, taking out and drying to obtain the carbon fiber nano-fabric.
Further preferably, the sandwich fabric can be prepared by using a paper sheet former, specifically: pouring the nanofiber into a standard paper sheet former, adding water, stirring for 3-10min to obtain nanofiber solution, stirring the cloth piece in the standard paper sheet former for 1-5min, opening, filtering, taking out, and drying to obtain the nanofiber fabric.
The nanofiber solution is an aqueous solution of nanofibers, and the mass concentration is 0.1 to 1%, more preferably 0.4%.
Preferably, in the felt in the step (1), the mass ratio of the total mass of the net tire and the carbon cloth to the sandwich cloth is 4-10:1, and more preferably 6:1.
Preferably, in the step (2), the mass ratio of the carbon fiber woven piece to the impregnating solution is 1: 5-20.
Preferably, in the step (2), the mass ratio of the solvent, the nanoparticles and the epoxy resin in the impregnation liquid is 20:1-2:1-2, and more preferably 20:1.6: 1.2.
Wherein the solvent is at least one selected from ethyl acetate, ethanol and acetone.
The nano particles are at least one of nano titanium dioxide and nano silicon dioxide, and the particle size is not more than 60 nm.
Preferably, in the step (2), the impregnation temperature is 68 ℃, and the impregnation time is 60 min.
Preferably, in the step (3), the drying includes, but is not limited to, natural airing, blow drying, drying and the like, and further preferably drying at 105 ℃.
The invention has the following beneficial effects:
(1) the prefabricated part can effectively improve the deposition speed of carbon atoms in the prefabricated material during vapor deposition, realize rapid densification and shorten the vapor deposition treatment time;
(2) the defect of mechanical property reduction caused by rapid densification is avoided, and the crucible prefabricated part prepared by the method can obtain good mechanical property and has long service life.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The present invention will be further explained with reference to specific examples in order to make the technical means, the technical features, the technical objectives and the effects of the present invention easier to understand, but the following examples are only preferred embodiments of the present invention, and not all embodiments of the present invention. In the interest of clarity, not all features of an actual implementation are described. In the following description, well-known functions or constructions are not described in detail since they would obscure the invention in unnecessary detail. It will of course be appreciated that in the development of any such actual embodiment, numerous implementation-specific details must be set forth in order to achieve the developer's specific goals. Based on the embodiments in the implementation, other embodiments obtained by those skilled in the art without any creative efforts belong to the protection scope of the present invention.
The experimental procedures in the following examples were carried out in a uniform and conventional manner unless otherwise specified, and materials, reagents and the like used in the following examples were commercially available unless otherwise specified.
In the embodiment described below, it is preferred that,
the nano titanium dioxide is purchased from titanium Tang nanotechnology, and the particle size is 5 nm;
the nano silicon dioxide is purchased from Jiangsu Tianxing New Material Co., Ltd, model TSP-H10, and has the particle size of 20 nm;
the epoxy resin is Dow DER 671;
the nano-fiber is purchased from nano-new material science and technology, article number 9112.
Basic embodiment
(1) Preparing a carbon fiber woven piece: weaving carbon fibers into a cloth piece, pouring the nanofibers into a standard paper sheet former, adding water, stirring for 5min to obtain a nanofiber solution with the mass concentration of 0.1-1%, wherein the mass ratio of the nanofibers to the carbon fibers is 1:40-80, stirring the cloth piece in the standard paper sheet former up and down for 3min, opening the water filter, filtering water, taking out and drying to obtain the sandwich cloth;
respectively weaving a mesh tire and carbon cloth by using carbon fiber raw materials, arranging an interlayer between the mesh tire and the carbon cloth, and compounding into a felt by needling, wherein the mass ratio of the total mass of the mesh tire and the carbon cloth to the mass of the interlayer cloth is 4-10: 1; winding the felt on a crucible mold, and overlapping and winding the needled carbon cloth and the net body until the density reaches 0.2-0.7g/cm3Obtaining a carbon fiber woven piece;
(2) dipping treatment: completely soaking the carbon fiber woven piece obtained in the step (1) in an impregnation liquid, wherein the mass ratio of the carbon fiber woven piece to the impregnation liquid is 1: 5-20, ultrasonic auxiliary treatment (ultrasonic power 1000W), wherein the impregnation liquid comprises a solvent, nano particles and epoxy resin, the impregnation temperature is 50-95 ℃, and the impregnation time is 30-150 min. And recovering the residual nanoparticles.
(3) And (3) drying the impregnated carbon fiber woven piece in a drying oven at 105 ℃ for 60min to obtain the carbon/carbon composite material crucible prefabricated piece.
Example 1
(1) Preparing a carbon fiber woven piece: weaving carbon fibers into a cloth piece, pouring the nanofibers into a standard paper sheet former, adding water and stirring for 5min to obtain a nanofiber solution with the mass concentration of 0.4%, wherein the mass ratio of the nanofibers to the carbon fibers is 1:50, vertically stirring the cloth piece in the standard paper sheet former for 3min, starting to filter water, filtering out water, taking out, and drying in an oven at 75 ℃ for 60min to obtain the sandwich cloth;
respectively weaving a mesh tire and carbon cloth by using carbon fiber raw materials, arranging an interlayer between the mesh tire and the carbon cloth, and compounding into a felt by needling, wherein the mass ratio of the total mass of the mesh tire and the carbon cloth to the mass of the interlayer cloth is 6: 1; winding the felt on a crucible mold, and then winding the needled carbon cloth and the net body in an overlapping manner at the densityReaches 0.39g/cm3Obtaining a carbon fiber woven piece;
(2) dipping treatment: completely soaking the carbon fiber woven piece obtained in the step (1) in an impregnation liquid, wherein the mass ratio of the carbon fiber woven piece to the impregnation liquid is 1: 10, carrying out ultrasonic auxiliary treatment (ultrasonic power is 1000W), and uniformly mixing and stirring the ethyl acetate, the nano titanium dioxide and the epoxy resin to obtain the impregnation liquid, wherein the mass ratio of the ethyl acetate to the nano titanium dioxide to the epoxy resin is 20:1.6:1.2, the impregnation temperature is 68 ℃, and the impregnation time is 60 min. And recovering the residual nanoparticles.
(3) And (3) drying the impregnated carbon fiber woven piece in a drying oven at 105 ℃ for 60min to obtain the carbon/carbon composite material crucible prefabricated piece.
Example 2
(1) Preparing a carbon fiber woven piece: weaving carbon fibers into a cloth piece, pouring the nanofibers into a standard paper sheet former, adding water and stirring for 5min to obtain a nanofiber solution with the mass concentration of 0.1%, wherein the mass ratio of the nanofibers to the carbon fibers is 1:40, vertically stirring the cloth piece in the standard paper sheet former for 3min, starting to filter water, filtering out water, taking out, and drying in an oven at 75 ℃ for 60min to obtain the sandwich cloth;
respectively weaving a mesh tire and carbon cloth by using carbon fiber raw materials, arranging an interlayer between the mesh tire and the carbon cloth, and compounding into a felt by needling, wherein the mass ratio of the total mass of the mesh tire and the carbon cloth to the mass of the interlayer cloth is 4: 1; winding the felt on a crucible mold, and overlapping and winding the needled carbon cloth and the net body until the density reaches 0.24g/cm3Obtaining a carbon fiber woven piece;
(2) dipping treatment: completely soaking the carbon fiber woven piece obtained in the step (1) in an impregnation liquid, wherein the mass ratio of the carbon fiber woven piece to the impregnation liquid is 1:5, carrying out ultrasonic auxiliary treatment (ultrasonic power is 1000W), wherein the impregnation liquid is prepared by uniformly mixing and stirring ethanol, nano titanium dioxide and epoxy resin, the mass ratio of the ethanol to the nano titanium dioxide to the epoxy resin is 20:1:1, the impregnation temperature is 68 ℃, and the impregnation time is 60 min. And recovering the residual nanoparticles.
(3) And (3) drying the impregnated carbon fiber woven piece in a drying oven at 105 ℃ for 60min to obtain the carbon/carbon composite material crucible prefabricated piece.
Example 3
(1) Preparing a carbon fiber woven piece: weaving carbon fibers into a cloth piece, pouring the nanofibers into a standard paper sheet former, adding water and stirring for 5min to obtain a nanofiber solution with the mass concentration of 1%, wherein the mass ratio of the nanofibers to the carbon fibers is 1:80, vertically stirring the cloth piece in the standard paper sheet former for 5min, starting to filter water, filtering out water, taking out, and drying in an oven at 75 ℃ for 60min to obtain the sandwich cloth;
respectively weaving a mesh tire and carbon cloth by using carbon fiber raw materials, arranging an interlayer between the mesh tire and the carbon cloth, and compounding into a felt by needling, wherein the mass ratio of the total mass of the mesh tire and the carbon cloth to the mass of the interlayer cloth is 10: 1; winding the felt on a crucible mold, and then overlapping and winding the needled carbon cloth and the net body to achieve the density of 0.57g/cm3Obtaining a carbon fiber woven piece;
(2) dipping treatment: completely soaking the carbon fiber woven piece obtained in the step (1) in an impregnation liquid, wherein the mass ratio of the carbon fiber woven piece to the impregnation liquid is 1:20, performing ultrasonic-assisted treatment (ultrasonic power is 1000W), and the impregnation liquid is prepared by uniformly mixing and stirring acetone, nano silicon dioxide and epoxy resin, wherein the mass ratio of the acetone, the nano silicon dioxide and the epoxy resin is 20:2:2, the impregnation temperature is 68 ℃, and the impregnation time is 60 min. And recovering the residual nanoparticles.
(3) And (3) drying the impregnated carbon fiber woven piece in a drying oven at 105 ℃ for 90min to obtain the carbon/carbon composite material crucible prefabricated piece.
Comparative example 1
Unlike example 1, comparative example 1 was not subjected to the impregnation treatment, i.e., the woven fabric of step (1) was prepared, and had a density of 0.41g/cm3。
Comparative example 2
In contrast to example 1, comparative example 2 had no sandwich cloth added and the knit density was 0.40g/cm3。
Comparative example 3
Different from the embodiment 1, the mass ratio of the total mass of the net tire and the carbon cloth to the sandwich cloth is 12:1, and the density of the weaving piece is 0.68g/cm3。
Comparative example 4
In contrast to example 1, the knit density was 0.46g/cm3Epoxy resin was not added to the impregnation solution.
Comparative example 5
In contrast to example 1, the knit density was 0.43g/cm3No nanoparticles were added to the impregnation solution.
Comparative example 6
In contrast to example 1, the knit density was 0.42g/cm3And the mass ratio of the ethyl acetate, the nano titanium dioxide and the epoxy resin in the impregnation liquid is 20:2.5: 0.5.
Comparative example 7
In contrast to example 1, the knit density was 0.83g/cm3。
Results testing
1. The crucible preforms prepared in examples and comparative examples were subjected to T-peel strength test according to a unified method, and the results are shown in table 1:
table 1.
2. Vapor deposition rate detection
The detection method comprises the following steps: respectively placing the prefabricated bodies prepared in the examples and the comparative examples on a supporting floor in a deposition furnace in an inverted mode, enabling an air mask on the supporting floor to be covered in a carbon fiber woven piece, and keeping the furnace pressure at 5 KPa;
firstly, setting the temperature in a furnace to be 850 ℃, using a carbon source of a mixed gas of methane, butylene and acetylene, wherein the volume ratio of the methane to the butylene to the acetylene in the mixed gas is 2:4:1, and the introduction amount of the mixed gas is 6m3Depositing for 80 hours, wherein the carrier gas is nitrogen, the volume ratio of the carrier gas to the carbon source is 2: 1;
then setting the temperature in the furnace to 1100 ℃, taking methane as a carbon source and 4m of methane as an inlet amount3And/h, the carrier gas is nitrogen, the volume ratio of the carrier gas to the carbon source is 2:1, the deposition is carried out for 50h, and the pressure difference between the inside and the outside of the crucible is controlled at 650 KPa.
Density change after vapor deposition was complete as in table 2:
table 2.
It can be seen that the strength of the preform of the present application is significantly improved, and at the same time, the nanoparticles adsorb in the woven article by a certain penetration, which greatly promotes the deposition of carbon atoms and improves the deposition efficiency.
The present invention is not limited to the above-described preferred embodiments, but rather, the present invention is to be construed broadly and cover all modifications, equivalents, and improvements falling within the spirit and scope of the present invention.
Claims (1)
1. A production process of a carbon/carbon composite crucible prefabricated part is characterized by comprising the following steps:
(1) preparing a carbon fiber woven piece: weaving carbon fibers into a cloth piece, pouring the nanofibers into a standard paper sheet former, adding water and stirring for 5min to obtain a nanofiber solution with the mass concentration of 0.4%, wherein the mass ratio of the nanofibers to the carbon fibers is 1:50, stirring the cloth piece up and down in the standard paper sheet former for 3min, starting to filter water, filtering out water, taking out, and drying in an oven at 75 ℃ for 60min to obtain the sandwich cloth; respectively weaving a mesh tire and carbon cloth by using carbon fiber raw materials, arranging an interlayer between the mesh tire and the carbon cloth, and compounding into a felt by needling, wherein the mass ratio of the total mass of the mesh tire and the carbon cloth to the mass of the interlayer cloth is 6: 1; winding the felt on a crucible mold, and then overlapping and winding the needled carbon cloth and the net body to achieve the density of 0.39g/cm3Obtaining a carbon fiber woven piece;
(2) dipping treatment: completely soaking the carbon fiber woven piece obtained in the step (1) in an impregnation liquid, wherein the mass ratio of the carbon fiber woven piece to the impregnation liquid is 1: 10, carrying out ultrasonic auxiliary treatment with ultrasonic power of 1000W, mixing and stirring uniformly the impregnation liquid by using ethyl acetate, nano titanium dioxide and epoxy resin, wherein the mass ratio of the ethyl acetate to the nano titanium dioxide to the epoxy resin is 20:1.6:1.2, the impregnation temperature is 68 ℃, the impregnation time is 60min, and the residual nano particles are recovered;
(3) and (3) drying the impregnated carbon fiber woven piece in a drying oven at 105 ℃ for 60min to obtain the carbon/carbon composite material crucible prefabricated piece.
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| CN112759409B (en) * | 2021-02-07 | 2022-01-14 | 内蒙古中晶科技研究院有限公司 | Carbon/carbon composite material vapor deposition process |
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| CN116409023A (en) * | 2021-12-30 | 2023-07-11 | 隆基绿能科技股份有限公司 | High-temperature-resistant carbon-carbon composite body, production method thereof and carbon fiber preform |
| 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 |
| CN117265641B (en) * | 2023-11-20 | 2024-01-30 | 内蒙古鼎泰万邦新材料有限公司 | Braided crucible preform and manufacturing method |
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