CN115594515A - Preparation method of corrosion-resistant carbon/carbon composite material heat-insulating cylinder based on winding process - Google Patents
Preparation method of corrosion-resistant carbon/carbon composite material heat-insulating cylinder based on winding process Download PDFInfo
- Publication number
- CN115594515A CN115594515A CN202211191379.XA CN202211191379A CN115594515A CN 115594515 A CN115594515 A CN 115594515A CN 202211191379 A CN202211191379 A CN 202211191379A CN 115594515 A CN115594515 A CN 115594515A
- Authority
- CN
- China
- Prior art keywords
- carbon
- composite material
- material heat
- corrosion
- insulating cylinder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 91
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 80
- 239000002131 composite material Substances 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 37
- 238000004804 winding Methods 0.000 title claims abstract description 31
- 230000007797 corrosion Effects 0.000 title claims abstract description 28
- 238000005260 corrosion Methods 0.000 title claims abstract description 28
- 230000008569 process Effects 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000000463 material Substances 0.000 claims abstract description 33
- 229920005989 resin Polymers 0.000 claims abstract description 33
- 239000011347 resin Substances 0.000 claims abstract description 33
- 238000002791 soaking Methods 0.000 claims abstract description 18
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000000919 ceramic Substances 0.000 claims abstract description 9
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 26
- 239000004917 carbon fiber Substances 0.000 claims description 26
- 239000010426 asphalt Substances 0.000 claims description 17
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 15
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 14
- 229920001568 phenolic resin Polymers 0.000 claims description 13
- 239000005011 phenolic resin Substances 0.000 claims description 13
- 239000000843 powder Substances 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 11
- 239000002243 precursor Substances 0.000 claims description 10
- WIEXMPDBTYDSQF-UHFFFAOYSA-N 1,3-bis(furan-2-yl)propan-2-one Chemical compound C=1C=COC=1CC(=O)CC1=CC=CO1 WIEXMPDBTYDSQF-UHFFFAOYSA-N 0.000 claims description 9
- 239000000805 composite resin Substances 0.000 claims description 8
- 239000012700 ceramic precursor Substances 0.000 claims description 6
- 238000003763 carbonization Methods 0.000 claims description 5
- 238000005087 graphitization Methods 0.000 claims description 5
- 239000003960 organic solvent Substances 0.000 claims description 5
- 238000007493 shaping process Methods 0.000 claims description 5
- 230000004048 modification Effects 0.000 claims description 4
- 238000012986 modification Methods 0.000 claims description 4
- 229920003257 polycarbosilane Polymers 0.000 claims description 4
- 229920001709 polysilazane Polymers 0.000 claims description 4
- DXZIFGZIQQRESB-UHFFFAOYSA-N [C].[Ti].[Si] Chemical group [C].[Ti].[Si] DXZIFGZIQQRESB-UHFFFAOYSA-N 0.000 claims description 3
- 238000002468 ceramisation Methods 0.000 claims description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 3
- 239000011863 silicon-based powder Substances 0.000 claims description 3
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 2
- ZQOBAJVOKBJPEE-UHFFFAOYSA-N [B].[C].[N].[Si] Chemical compound [B].[C].[N].[Si] ZQOBAJVOKBJPEE-UHFFFAOYSA-N 0.000 claims description 2
- 238000010000 carbonizing Methods 0.000 claims description 2
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 2
- 230000007480 spreading Effects 0.000 claims description 2
- 238000003892 spreading Methods 0.000 claims description 2
- 238000009736 wetting Methods 0.000 claims 1
- 229910052710 silicon Inorganic materials 0.000 abstract description 10
- 239000010703 silicon Substances 0.000 abstract description 10
- 239000011159 matrix material Substances 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000000465 moulding Methods 0.000 abstract 1
- 230000002035 prolonged effect Effects 0.000 abstract 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 11
- 238000004321 preservation Methods 0.000 description 8
- 239000000835 fiber Substances 0.000 description 6
- 230000004584 weight gain Effects 0.000 description 6
- 235000019786 weight gain Nutrition 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- 230000002787 reinforcement Effects 0.000 description 5
- 239000002994 raw material Substances 0.000 description 3
- 238000004046 wet winding Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- XHLBZCSWZFBXDD-UHFFFAOYSA-N C=O.C1(=CC=CC=C1)O.[B] Chemical compound C=O.C1(=CC=CC=C1)O.[B] XHLBZCSWZFBXDD-UHFFFAOYSA-N 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- KWGASIUWELSTHP-UHFFFAOYSA-N boron;phenol Chemical compound [B].OC1=CC=CC=C1 KWGASIUWELSTHP-UHFFFAOYSA-N 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- 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
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- 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
- C04B35/515—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
- C04B35/522—Graphite
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- 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
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- 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
- C04B2235/656—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
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- 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
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/77—Density
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- 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
- C04B2235/70—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
- C04B2235/9669—Resistance against chemicals, e.g. against molten glass or molten salts
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Composite Materials (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Ceramic Products (AREA)
Abstract
The invention relates to a preparation method of a corrosion-resistant carbon/carbon composite material heat-insulating cylinder based on a winding process. Compared with the prior art, the method can realize the rapid molding preparation of the heat-insulating cylinder, is not limited by large size, has simple process and few working procedures, and is beneficial to improving the production efficiency of the heat-insulating cylinder and improving the productivity; the ceramic resin or modified resin soaking material is selected to generate a ceramic phase in the matrix of the heat-insulating cylinder product, so that silicon steam corrosion in the use process can be effectively avoided, and the service life of the product is prolonged.
Description
Technical Field
The invention belongs to the technical field of carbon/carbon composite material heat-insulating cylinders, and relates to a preparation method of a corrosion-resistant carbon/carbon composite material heat-insulating cylinder based on a winding process.
Background
At present, the global photovoltaic industry develops at a high speed, the productivity of monocrystalline silicon is accelerated, and a pulling method used for producing the monocrystalline silicon needs to be carried out in a monocrystalline silicon furnace. The high demand for the productivity of single crystal silicon will lead to a dramatic increase in the number of single crystal silicon furnaces and a trend toward larger sizes. As a consumable material in a monocrystalline silicon furnace, the consumable material occupies about 9% of the production cost of the whole monocrystalline silicon. Along with the requirements of newly-added monocrystalline silicon furnaces, large-size transformation requirements and original replacement requirements, thermal field components mainly comprising a crucible, a guide cylinder, a heat-insulating cylinder and a heater are gradually in short supply. The heat preservation cylinder is used for preventing heat in the monocrystalline silicon furnace from being conducted to the outside, and plays a very critical role in ensuring the thermal field environment of the monocrystalline silicon furnace. Carbon/carbon composite materials are formed using carbon as a matrix and carbon fiber preforms as reinforcement, and have both a low density of carbon materials and a high strength of fibers, and have recently been replacing graphite and becoming a material for thermal field components with a relatively high cost performance.
Manufacturers of carbon/carbon composite material thermal field components usually select a Chemical Vapor Infiltration (CVI) process, and different types and sizes of thermal field products are uniformly placed in a Deposition furnace in a nested manner to prepare the thermal field products in order to save cost and improve productivity. For the CVI process, the preparation period is long, and the CVI furnace has the defect of large-size limitation; for the heat preservation cylinder, as the size of the single crystal silicon furnace is increased, the size of the heat preservation cylinder is gradually changed from 32 inches which is commonly used before to 36 inches, compared with other thermal field components, the heat preservation cylinder has the largest volume, and the heat preservation cylinder is usually placed at the outermost edge position of a CVI furnace chamber in the preparation process, so that a large part of heat is isolated from other components, and the capacity of other thermal field matching products is severely limited.
The carbon/carbon composite material heat-insulating cylinder mainly takes a carbon fiber needled felt as a reinforcement, holes can be left in the Z direction of the reinforcement in the needling process, in a use environment, the carbon can react with silicon steam generated due to high temperature to be consumed, and the Z-direction needled holes increase diffusion channels of the silicon steam, even the fiber reinforcement is damaged, so that the carbon/carbon composite material heat-insulating cylinder is cracked, deformed and loses efficacy.
The present invention is proposed to solve the above-mentioned drawbacks.
Disclosure of Invention
The invention aims to provide a preparation method of a corrosion-resistant carbon/carbon composite material heat-insulating cylinder based on a winding process.
The invention adopts a wet winding process to prepare the carbon fiber soaked with the resin into a prefabricated body in the shape of a heat preservation cylinder, the prefabricated body is solidified to form the resin-based composite material heat preservation cylinder, and the resin-based composite material heat preservation cylinder is obtained after subsequent carbonization and high-temperature treatment. The fiber reinforcement and the matrix raw material are integrally formed by a full-automatic fiber wet winding process; after the resin impregnating solution is subjected to component design and modification, the carbon residue rate and the corrosion resistance of a matrix can be obviously improved. The process method has the advantages of high efficiency, low cost and the like, and provides technical possibility for the rapid preparation of large-size carbon/carbon composite material heat-insulating cylinders and other thermal field products.
The purpose of the invention can be realized by the following technical scheme:
a preparation method of a corrosion-resistant carbon/carbon composite material heat-insulating cylinder based on a winding process comprises the following steps:
(1) Preparing precursor resin and an organic solvent into a soaking material, and gradually soaking continuous carbon fibers in the soaking material;
(2) Spreading the soaked carbon fibers on the surface of the core mold, and curing and shaping to obtain a resin-based composite material heat-insulating cylinder;
(3) Carbonizing a resin-based composite material heat-insulating cylinder to obtain a carbon/carbon composite material heat-insulating cylinder;
(4) And carrying out ceramic treatment and high-temperature graphitization treatment on the carbon/carbon composite material heat-insulating cylinder to obtain the corrosion-resistant carbon/carbon composite material heat-insulating cylinder, namely the target product.
Further, the precursor resin is phenolic resin, furfuryl ketone resin, a phenolic resin/asphalt mixture or a furfuryl ketone resin/asphalt mixture.
Furthermore, in the phenolic resin/asphalt mixture, the weight ratio of the phenolic resin to the asphalt is 10: (0-5), and the asphalt is not 0;
in the furfuryl ketone resin/asphalt mixture, the weight ratio of the furfuryl ketone resin to the asphalt is 10: (0-5), and the asphalt is not 0.
Furthermore, before the precursor resin is prepared into the soaking material, powder or ceramic precursor is also adopted for doping, mixing and modifying. Furthermore, the powder is titanium silicon carbon powder, silicon boron carbon nitrogen powder, silicon nitride powder or a mixture of silicon carbide, silicon powder and carbon powder.
Furthermore, the ceramic precursor is polycarbosilane, polysilazane or polysilaborazane.
Furthermore, the doping weight ratio of the powder or the ceramic precursor is 5-30%.
Further, the precursor resin can be selected from boron phenol formaldehyde resin capable of being ceramized.
Further, the organic solvent may be ethanol, acetone, or the like.
Further, in the step (1), the mass ratio of the precursor resin to the organic solvent is 5 to 20.
Furthermore, in the step (1), the speed of soaking the carbon fibers in the soaking material is 0.5-2 m/s.
Further, in the step (2), in the laying process, the winding tension of the carbon fiber is 50N-100N, and the carbon fiber tension gradually decreases with the increase of the thickness of the laying layer, specifically, the winding tension of the laying layer contacting with the core mold is 100N, and the fiber tension can gradually decrease to about 50N with the increase of the thickness of the laying layer (except for the outermost carbon fiber).
Further, in the step (2), in the layering process, the winding angle of the carbon fiber is 0-90 degrees, and the winding angles of the carbon fiber of the innermost layer and the carbon fiber of the outermost layer are different from those of the carbon fiber of the middle layer.
Further, in the step (2), the temperature for curing and shaping is between room temperature and 300 ℃, and the time is 1-10 h.
Further, in the step (3), the temperature of the carbonization treatment is 500-1000 ℃, and the time is 50-100 h.
Furthermore, in the step (4), the ceramic temperature is 1000-1800 ℃ and the time is 10-50 h.
Further, in the step (4), the graphitization temperature is 1800-2200 ℃ and the time is 1-10 h.
Compared with the prior art, the invention has the following advantages:
1. according to the invention, the rapid forming preparation of the heat-insulating cylinder can be realized through a fiber wet winding process, and the method is not limited by large size;
2. the process for preparing the carbon/carbon composite material heat-insulating cylinder is simple and easy, has few working procedures, and is beneficial to improving the production efficiency of the heat-insulating cylinder and the productivity;
3. the ceramic resin or modified resin soaking material selected by the invention can generate a ceramic phase in the matrix of the heat-insulating cylinder product, can effectively avoid silicon vapor corrosion in the using process and prolong the service life of the product.
Detailed Description
The present invention will be described in detail with reference to specific examples. The present embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, but the scope of the present invention is not limited to the following embodiments.
In the following examples, the raw materials such as boron phenol resin, furfuryl ketone resin, polysilazane, polycarbosilane, polysilazane and the like were directly purchased as commercial products, and specifically purchased from manufacturers and units including national defense science and technology university, kubei chemical, and denz spring.
Otherwise, unless otherwise specified, all the conventional commercial raw materials or conventional processing techniques are used in the art.
Example 1:
in this embodiment, the efficient preparation process method of the corrosion-resistant carbon/carbon composite material heat-insulating cylinder based on the winding process includes the following steps:
a. selecting a 32-inch core mold for preparing a 32-inch carbon/carbon composite material heat-insulating cylinder with the thickness of 15 mm;
b. selecting boron phenolic resin as a precursor, and preparing a resin soaking material by using absolute ethyl alcohol, wherein the adding amount ratio of the resin to the absolute ethyl alcohol is 5 g;
c. adopting continuous carbon fibers, and gradually infiltrating the continuous carbon fibers into the boron phenolic resin impregnating material from the speed of 1 m/s;
d. under the tension of 100N and the winding angle of 90 degrees, the carbon fiber soaked with the resin finishes a first layer of winding and layering on the surface of the core mold; then, continuously layering at a winding angle of 60 degrees and a tension decreasing till 60N until the thickness approaches 15mm, finishing the last layer of winding layer at a tension of 100N and a winding angle of 90 degrees, and curing and shaping at a temperature of 80 ℃ to obtain a 32-inch resin-based composite material heat-insulating cylinder with the thickness of 15 mm;
e. carrying out carbonization treatment on the resin-based composite material at 800 ℃ for 70h to obtain a carbon/carbon composite material heat-insulating cylinder;
f. and carrying out ceramic treatment at 1400 ℃ and graphitization treatment at 1850 ℃ on the carbon/carbon composite material heat-insulating cylinder to finally obtain a finished product.
The density of the finally obtained carbon/carbon composite material heat-preserving barrel is 1.2g/cm 3 About, the corrosion weight gain under the silicon steam environment can be guaranteed to be less than 15%, and the carbon residue rate of the resin impregnating material is about 60%.
Example 2:
this example is substantially the same as example 1 except that:
in this example, 10wt% of titanium silicon carbon powder is doped with modified phenolic resin as a soaking material, and the ceramization temperature is 1450 ℃.
The density of the finally obtained carbon/carbon composite material heat-preserving barrel is 1.4g/cm 3 About, the corrosion weight gain under the silicon steam environment can be guaranteed to be less than 10%, and the carbon residue rate of the resin impregnating material is about 55%.
Example 3:
this embodiment is substantially the same as embodiment 1 described above, except that:
phenolic resin modified by 5wt% of silicon powder, 5wt% of carbon powder and 5wt% of silicon carbide powder is selected as a soaking material, and the ceramic temperature is 1600 ℃.
The density of the finally obtained carbon/carbon composite material heat-preserving barrel is 1.4g/cm 3 About, the corrosion weight gain under the silicon steam environment can be guaranteed to be less than 5%, and the carbon residue rate of the resin impregnating material is about 65%.
Example 4:
this embodiment is substantially the same as embodiment 1 described above, except that:
10wt% of polyborosilazane doped and modified phenolic resin is selected as a soaking material, the curing temperature is 250 ℃, and the ceramization temperature is 1000 ℃.
The density of the finally obtained carbon/carbon composite material heat-preserving barrel is 1.3g/cm 3 About, the corrosion weight gain under the silicon steam environment can be guaranteed to be less than 5%, and the carbon residue rate of the resin impregnating material is about 60%.
Example 5:
this embodiment is substantially the same as embodiment 1 described above, except that:
selecting 10wt% polycarbosilane doped and modified 65wt% phenolic resin-35 wt% asphalt mixture as a soaking material, wherein the carbonization temperature is 1000 ℃.
The density of the finally obtained carbon/carbon composite material heat-insulating barrel is 1.4g/cm 3 About, the corrosion weight gain under the silicon steam environment can be guaranteed to be less than 5%, and the carbon residue rate of the resin impregnating material is about 70%.
Comparative example 1:
compared to example 3, most of them are identical, except that the phenolic resin is not modified by doping.
The density of the finally obtained carbon/carbon composite material heat-preserving barrel is 1.2g/cm 3 On the other hand, the corrosion weight gain in the silicon vapor environment can only be guaranteed to be less than 20%, and the carbon residue rate of the resin impregnating material is about 40%.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (10)
1. A preparation method of a corrosion-resistant carbon/carbon composite material heat-insulating cylinder based on a winding process is characterized by comprising the following steps:
(1) Preparing precursor resin and an organic solvent into a soaking material, and gradually soaking continuous carbon fibers in the soaking material;
(2) Spreading the soaked carbon fibers on the surface of the core mold, and curing and shaping to obtain a resin-based composite material heat-insulating cylinder;
(3) Carbonizing the resin-based composite material heat-insulating cylinder to obtain a carbon/carbon composite material heat-insulating cylinder;
(4) And carrying out ceramic treatment and high-temperature graphitization treatment on the carbon/carbon composite material heat-insulating cylinder to obtain the corrosion-resistant carbon/carbon composite material heat-insulating cylinder, namely the target product.
2. The preparation method of the corrosion-resistant carbon/carbon composite material heat-insulating cylinder based on the winding process as claimed in claim 1, wherein the precursor resin is phenolic resin, furfuryl ketone resin, phenolic resin \ asphalt mixture or furfuryl ketone resin \ asphalt mixture.
3. The preparation method of the corrosion-resistant carbon/carbon composite material heat-insulating cylinder based on the winding process as claimed in claim 2, wherein in the phenolic resin/asphalt mixture, the weight ratio of phenolic resin to asphalt is 10: (0-5), and the asphalt is not 0;
in the furfuryl ketone resin/asphalt mixture, the weight ratio of the furfuryl ketone resin to the asphalt is 10: (0-5), and the asphalt is not 0.
4. The preparation method of the corrosion-resistant carbon/carbon composite material heat-insulating cylinder based on the winding process as claimed in claim 1, wherein the precursor resin is subjected to doping modification by using powder or ceramic precursor before being prepared into a wetting material, wherein the powder is titanium silicon carbon powder, silicon boron carbon nitrogen powder, silicon nitride powder or silicon carbide, silicon powder or carbon powder mixture;
the ceramic precursor is polycarbosilane, polysilazane or polysilaborazane;
the doping weight ratio of the powder or the ceramic precursor is 5-30%.
5. The preparation method of the corrosion-resistant carbon/carbon composite material heat-preserving cylinder based on the winding process as claimed in claim 1, wherein in the step (1), the mass ratio of the precursor resin to the organic solvent is (5-20): 100.
6. the preparation method of the corrosion-resistant carbon/carbon composite material heat-insulating cylinder based on the winding process as claimed in claim 1, wherein in the step (1), the speed of soaking the carbon fibers in the soaking material is 0.5-2 m/s.
7. The preparation method of the corrosion-resistant carbon/carbon composite material heat-preserving cylinder based on the winding process as claimed in claim 1, wherein in the step (2), the winding tension of the carbon fibers is 50N-100N in the layering process, and the tension of the carbon fibers is gradually reduced with the increase of the thickness of the layering except for the outermost carbon fibers; the winding angle of the carbon fiber is 0-90 degrees, and the winding angle of the innermost carbon fiber and the winding angle of the outermost carbon fiber are different from the winding angle of the intermediate carbon fiber.
8. The preparation method of the corrosion-resistant carbon/carbon composite material heat-preserving cylinder based on the winding process as claimed in claim 1, wherein in the step (2), the temperature for curing and shaping is from room temperature to 300 ℃ for 1-10 h.
9. The method for preparing the corrosion-resistant carbon/carbon composite material heat-preserving cylinder based on the winding process as claimed in claim 1, wherein in the step (3), the temperature of the carbonization treatment is 500-1000 ℃ and the time is 50-100 h.
10. The preparation method of the corrosion-resistant carbon/carbon composite material heat-preserving cylinder based on the winding process as claimed in claim 1, wherein in the step (4), the temperature of ceramization is 1000-1800 ℃ and the time is 10-50 h;
the temperature of graphitization is 1800-2200 ℃ and the time is 1-10 h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211191379.XA CN115594515A (en) | 2022-09-28 | 2022-09-28 | Preparation method of corrosion-resistant carbon/carbon composite material heat-insulating cylinder based on winding process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211191379.XA CN115594515A (en) | 2022-09-28 | 2022-09-28 | Preparation method of corrosion-resistant carbon/carbon composite material heat-insulating cylinder based on winding process |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115594515A true CN115594515A (en) | 2023-01-13 |
Family
ID=84844426
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211191379.XA Pending CN115594515A (en) | 2022-09-28 | 2022-09-28 | Preparation method of corrosion-resistant carbon/carbon composite material heat-insulating cylinder based on winding process |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115594515A (en) |
-
2022
- 2022-09-28 CN CN202211191379.XA patent/CN115594515A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110105075B (en) | High-purity carbon fiber reinforced silicon carbide composite material and preparation method thereof | |
| US8454867B2 (en) | CVI followed by coal tar pitch densification by VPI | |
| US8268207B2 (en) | Densification of C-C composites with pitches followed by CVI/CVD | |
| CN113816757A (en) | Method for quickly preparing carbon-carbon composite material heat-insulating barrel | |
| CN105541364B (en) | A kind of method of step densification production carbon pottery automobile brake disc | |
| CN116143537B (en) | Composite carbon-carbon crucible containing antioxidant coating and preparation method thereof | |
| CN113149686B (en) | Carbon/carbon composite material crucible with composite ceramic layer and preparation method thereof | |
| CN112299865A (en) | A kind of modified C/SiC composite material and preparation method thereof | |
| JP2025507648A (en) | High-strength carbon/ceramic brake disc with ceramic functional layer | |
| CN112110743A (en) | CVI, PIP and RMI combined process for preparing carbon/carbon ceramic composite material brake disc | |
| CN113173791B (en) | SiBCN interface coating for SiC fiber reinforced composite material, and preparation method and application thereof | |
| CN113121253B (en) | Ultrahigh-temperature C/SiHfBCN ceramic matrix composite material and preparation method thereof | |
| CN119638467A (en) | Mesophase pitch carbon matrix modified high-heat-conductivity C/SiC composite material and preparation method thereof | |
| CN119143514A (en) | Carbon/carbon-silicon carbide gradient composite material sagger and preparation method and application thereof | |
| CN114455969A (en) | High-density C/C-SiC composite material crucible containing aluminum oxide coating | |
| CN115594515A (en) | Preparation method of corrosion-resistant carbon/carbon composite material heat-insulating cylinder based on winding process | |
| CN115991608B (en) | Preparation method of endogenous fiber reinforced carbon/Tao Hou lining material | |
| CN116143109B (en) | A carbon nanotube/graphene/pyrolytic carbon composite material and preparation method thereof | |
| CN113526971B (en) | Method for preparing SiC ceramic matrix composite material from spongy silicon carbide nanofiber preform | |
| CN114411242A (en) | Quartz fiber reinforced carbon-silicon dioxide composite material guide cylinder and preparation method thereof | |
| CN114105665A (en) | Light carbon/carbon composite material heat-insulating cylinder for crystalline silicon and preparation method thereof | |
| CN113735596A (en) | Nitride fiber reinforced composite material and preparation method and application thereof | |
| CN115745646B (en) | Preparation method of carbon/carbon composite material | |
| CN117105678B (en) | High-compactness carbon ceramic barrel and preparation method thereof | |
| CN112110748A (en) | Preparation method of two-dimensional high-thermal-conductivity C/C-ZrC-SiC composite material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication |