CN113816757A - Method for quickly preparing carbon-carbon composite material heat-insulating barrel - Google Patents
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Abstract
The invention relates to the field of composite materials, and discloses a method for quickly preparing a carbon-carbon composite heat-insulating barrel, aiming at the problems of long production period, complex process and low efficiency of the heat-insulating barrel in the prior art, the following scheme is proposed, which comprises the following steps: s1, preparing a carbon fiber preform: alternately laminating and needling the mesh tire, the carbon cloth and the carbon fiber yarn which are made of the carbon fiber into a prefabricated body with the required size, and carrying out high speed and high speed double-row cultivation with the density of 0.4 g/cm-0.5 g/cm; s2, hardening: spraying glue solution on the surface of the preform needled in the step S1 by using a spray gun, wherein the glue solution is mixed solution of FB phenolic resin and NL type curing agent in a proportion of 8-12%, and airing at room temperature for 8-20 h after spraying is finished to harden. The invention abandons the traditional deposition process, and selects the impregnation carbonization process with shorter densification period and lower cost; compared with the finished product produced by the deposition process, the finished product produced by the production process has stable quality and better density uniformity of the heat-insulating cylinder.
Description
Technical Field
The invention relates to the field of composite materials, in particular to a method for quickly preparing a carbon-carbon composite material heat-insulating barrel.
Background
Carbon/carbon composites are carbon matrix composites reinforced with carbon fibers and fabrics thereof. Has a low density of<2.0g/cm3) High strength, high specific modulus, high thermal conductivity, low expansion coefficient, good friction performance, good thermal shock resistance and high dimensional stabilityAnd the like, which are a few candidate materials applied above 1650 ℃ nowadays, the highest theoretical temperature is as high as 2600 ℃, and therefore the material is considered to be one of the most promising high-temperature materials. The material is prepared by compounding a mesh tire made of carbon fibers, carbon cloth and carbon fiber yarns into a carbon fiber preform by alternately laminating and needling, then putting the preform into a chemical vapor reaction furnace, and carrying out chemical vapor densification on the preform by utilizing pyrolytic carbon generated by pyrolysis of carbon source gas at high temperature or utilizing resin carbon generated after resin liquid phase impregnation and carbonization so as to gradually increase the density of the carbon fiber preform to form the carbon/carbon composite material. 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.
At present, the carbon/carbon composite material is widely applied to the high-temperature field of a single crystal furnace and is used for manufacturing thermal field parts, such as a crucible, a heat shield, a heat-preserving barrel, a crucible support, fastening screws and the like. The traditional preparation method of the heat-insulating barrel is that carbon fibers, net tires and carbon cloth are alternately laminated and needled to form a prefabricated body, and the prefabricated body is deposited, impregnated, cured, carbonized, subjected to high-temperature treatment and machined to reach the required finished product size. However, in terms of cost and efficiency, the densification speed of the deposition process is far less than that of impregnation carbonization, and particularly, the deposition efficiency is lower when the product density is more than 1.0g/cm during the process of carrying out the high-density carbon fiber by the method. The period of each furnace of the deposition process is 200-300 hours, the period of each furnace is basically more than 20 days by adding the time of temperature rise and temperature reduction, the density of products discharged from the furnace is often less than 1.3g/cm, machining and turning to remove blocked pores on the surface of a blank preform for further densification, then returning to the furnace for secondary deposition, and thus the requirement of finished products can be met after one period of deposition. Therefore, the production cycle of each product is at least more than 45 days by adding the high-temperature treatment time in the later period, and a large amount of waste is caused in consideration of the production time and the manufacturing cost.
Disclosure of Invention
The invention provides a method for quickly preparing a carbon-carbon composite material heat-insulating barrel, which solves the problems of long production cycle, complex process and low efficiency of the heat-insulating barrel in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for quickly preparing a carbon-carbon composite material heat-insulating barrel comprises the following steps:
s1, preparing a carbon fiber preform: alternately laminating and needling the mesh tire, the carbon cloth and the carbon fiber yarn which are made of the carbon fiber into a prefabricated body with the required size, and carrying out high speed and high speed double-row cultivation with the density of 0.4 g/cm-0.5 g/cm;
s2, hardening: spraying glue solution on the surface of the preform needled in the S1 by using a spray gun, wherein the glue solution is mixed solution of FB phenolic resin and NL type curing agent in a proportion of 8-12%, and after the spraying is finished, airing the preform at room temperature for 8-20 h to harden the preform;
s3, densification: placing the well hardened carbon-carbon composite material heat-insulating cylinder preform in the step S2 in an impregnation furnace, impregnating and curing the preform by using furan resin, wherein the curing temperature is 120-180 ℃, the time is 6-10 hours, the cured product is carbonized at a low temperature, the final temperature of the low-temperature carbonization is 600 ℃, the weight is weighed after the carbonization to calculate the density, the impregnation, the curing and the carbonization are continued if the density is less than 1.3g/cm, and the density of the carbon-carbon composite material heat-insulating cylinder obtained after 2-3 cycles of densification is larger than 1.3 g/cm;
s4, high-temperature graphitization: putting the carbon-carbon composite material heat-insulating cylinder prepared in the S3 into a high-temperature furnace for high-temperature purification treatment, wherein the graphitization temperature is 2000-2300 ℃, and the graphitization time is 20-30 h;
s5, machining: and (4) processing the carbon-carbon composite material heat-insulating cylinder obtained after high-temperature graphitization in S4 into a carbon-carbon composite material heat-insulating cylinder finished product with the final size according to the shape and size required by the finished product.
Preferably, the carbon fiber filaments in the S1 step are 12K tow fibers.
Preferably, in the step S2, the FB phenolic resin and the NL curing agent are mixed by slowly pouring the curing agent into the phenolic resin while stirring the phenolic resin, so that the curing agent is uniformly mixed, and the curing agent is not poured violently to cause the phenolic resin to be instantly and locally cured.
Preferably, nitrogen is used for pressurization in the impregnation and curing processes in the step S3 to improve densification efficiency, the carbonization process is normal pressure carbonization, the whole temperature increase and decrease process is carried out in a nitrogen atmosphere, the temperature of the last carbonization is 900 ℃, the rest carbonization temperatures are 600 ℃, and the carbonization time is 24-48 h.
Preferably, the high-temperature graphitization process in the step S4 is as follows: continuously heating in a vacuum state, continuously vacuumizing in the whole heating process, filling nitrogen to normal pressure after heating is finished, and performing machining treatment after cooling to room temperature.
In the invention:
compared with the prior art, the invention has the following advantages:
1. compared with the existing deposition process, the energy consumption of auxiliary materials and equipment in the impregnation carbonization process is far less than that of the deposition process under the condition of adding carbon with the same weight;
2. compared with the prior deposition process period, the hardening-impregnating-curing-carbonizing process has shorter time, so that the production efficiency can be better improved, and the production cost is reduced;
in conclusion, the rapid preparation method of the carbon-carbon composite material heat-insulating cylinder provided by the invention abandons the traditional deposition process, has a shorter densification period and a lower cost and is a dipping carbonization process; compared with the finished product produced by the deposition process, the finished product produced by the production process has stable quality and better density uniformity of the heat-insulating cylinder.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
With reference to FIG. 1
Example 1:
a method for quickly preparing a carbon-carbon composite material heat-insulating barrel comprises the following steps:
s1: preparing a prefabricated body, namely alternately laminating and needling a mesh tire, carbon cloth and carbon fiber yarns which are made of carbon fibers into the prefabricated body with the required size, wherein the density of the prefabricated body is 0.45g/cm for carrying out heavy planting, and the carbon fiber yarns are 12K tow fibers;
s2: hardening the preform, namely spraying glue solution on the surface of the preform needled in the step 1 by using a spray gun, wherein the proportion of the glue solution is 8 percent of FB phenolic resin and NL type curing agent, and airing at 25 ℃ for 10 hours after spraying is finished to harden the preform;
s3: densifying, namely putting the heat-insulating barrel preform hardened in the step S2 into an impregnation and solidification integrated furnace for impregnating resin to densify, wherein an impregnating solution is high-carbon-residue furan resin and a sulfonic acid curing agent, the proportion of the curing agent is 3%, putting the cured heat-insulating barrel into a carbonization furnace for low-temperature carbonization, the carbonization temperature is 600 ℃, the carbonization time is 30h, continuously circulating the densification process in the step 3 for 2 cycles after carbonization, and then obtaining the carbon-carbon composite material heat-insulating barrel with the density of 1.35 g/cm;
s4: performing high-temperature graphitization, namely performing high-temperature graphitization on the heat-insulating barrel carbonized in the step S3, wherein the graphitization temperature is 2300 ℃, the time is 24 hours, and the ash content of the heat-insulating barrel after graphitization is less than 200 ppm;
s5: and (4) machining, namely machining the carbon-carbon composite material heat-insulating cylinder obtained after high-temperature graphitization in S4 into a carbon-carbon composite material heat-insulating cylinder finished product with the final size according to the shape and size required by the finished product.
Example 2:
a method for quickly preparing a carbon-carbon composite material heat-insulating barrel comprises the following steps:
s1: preparing a prefabricated body, namely alternately laminating and needling a mesh tire, carbon cloth and carbon fiber yarns which are made of carbon fibers into the prefabricated body with the required size, wherein the density of the prefabricated body is 0.5g/cm for carrying out heavy planting, and the carbon fiber yarns are 12K tow fibers;
s2: hardening the preform, namely spraying glue solution on the surface of the preform needled in the step 1 by using a spray gun, wherein the proportion of the glue solution is 12 percent of FB phenolic resin and NL type curing agent, and airing at 25 ℃ for 8 hours after spraying is finished to harden the preform;
s3: densifying, namely putting the heat-insulating barrel preform hardened in the step S2 into an impregnation and solidification integrated furnace for impregnating resin to densify, wherein an impregnating solution is high-carbon-residue furan resin and a sulfonic acid curing agent, the proportion of the curing agent is 3%, putting the cured heat-insulating barrel into a carbonization furnace for low-temperature carbonization, the carbonization temperature is 600 ℃, the carbonization time is 30 hours, continuously circulating the densification process in the step 3 for 2 periods after carbonization, the carbonization temperature of the first two times is 600 ℃, the temperature of the last time is 900 ℃, and obtaining the carbon-carbon composite heat-insulating barrel with the density of 1.4 g/cm;
s4: performing high-temperature graphitization, namely performing high-temperature graphitization on the heat-insulating barrel carbonized in the S3, wherein the graphitization temperature is 2200 ℃, the time is 24 hours, and the ash content of the heat-insulating barrel after graphitization is less than 200 ppm;
s5: and (4) machining, namely machining the carbon-carbon composite material heat-insulating cylinder obtained after high-temperature graphitization in S4 into a carbon-carbon composite material heat-insulating cylinder finished product with the final size according to the shape and size required by the finished product.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (5)
1. A method for quickly preparing a carbon-carbon composite material heat-insulating barrel is characterized by comprising the following steps:
s1, preparing a carbon fiber preform: alternately laminating and needling the mesh tire, the carbon cloth and the carbon fiber yarn which are made of the carbon fiber into a prefabricated body with the required size, and carrying out high speed and high speed double-row cultivation with the density of 0.4 g/cm-0.5 g/cm;
s2, hardening: spraying glue solution on the surface of the preform needled in the step S1 by using a spray gun, wherein the glue solution is mixed solution of FB phenolic resin and NL type curing agent in a proportion of 8-12%, and after the spraying is finished, airing the preform at room temperature for 8-20 h to harden the preform;
s3, densification: placing the hardened carbon-carbon composite material heat-insulating cylinder preform in the step S2 in an impregnation furnace, impregnating and curing the preform with furan resin, wherein the curing temperature is 120-180 ℃ and the time is 6-10 h, performing low-temperature carbonization on the cured product, the final temperature of the low-temperature carbonization is 600 ℃, weighing the weight after carbonization to calculate the density, continuing impregnation and curing carbonization if the density is less than 1.3g/cm, and carrying out densification for 2-3 periods to obtain a carbon-carbon composite material heat-insulating cylinder with the density more than 1.3 g/cm;
s4, high-temperature graphitization: putting the carbon-carbon composite material heat-insulating cylinder prepared in the step S3 into a high-temperature furnace for high-temperature purification treatment, wherein the graphitization temperature is 2000-2300 ℃, and the graphitization time is 20-30 h;
s5, machining: and (4) processing the carbon-carbon composite material heat-insulating cylinder obtained after high-temperature graphitization in the step S4 into a carbon-carbon composite material heat-insulating cylinder finished product with the final size according to the shape and size required by the finished product.
2. The method for rapidly manufacturing the carbon-carbon composite material heat-preserving barrel according to claim 1, wherein the carbon fiber filaments in the step S1 are 12K tow fibers.
3. The method for rapidly manufacturing a carbon-carbon composite thermal insulation barrel according to claim 1, wherein in the step S2, the FB phenolic resin and the NL curing agent are mixed by slowly pouring the curing agent into the phenolic resin while stirring the phenolic resin, so that the curing agent is uniformly mixed, and the curing agent is not poured violently to cause instantaneous partial curing of the phenolic resin.
4. The method for rapidly preparing the carbon-carbon composite heat-preserving container as claimed in claim 1, wherein the impregnation and curing in the step S3 are performed by pressurizing with nitrogen to increase the densification efficiency, the carbonization process is performed under normal pressure, the whole temperature increase and decrease process is performed in nitrogen atmosphere, the temperature of the last carbonization is 900 ℃, the rest carbonization temperatures are 600 ℃, and the carbonization time is 24-48 h.
5. The method for rapidly preparing the carbon-carbon composite material heat-preserving container according to claim 1, wherein the high-temperature graphitization process in the step S4 is as follows: continuously heating in a vacuum state, continuously vacuumizing in the whole heating process, filling nitrogen to normal pressure after heating is finished, and performing machining treatment after cooling to room temperature.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114436670A (en) * | 2022-03-09 | 2022-05-06 | 西安美兰德新材料有限责任公司 | Winding forming-based high-strength carbon-carbon cylinder preparation method |
| CN115231940A (en) * | 2022-08-01 | 2022-10-25 | 青岛晶易新材料科技股份有限公司 | Production process of carbon thermal insulation cylinder |
| CN115231939A (en) * | 2022-07-22 | 2022-10-25 | 青岛晶易新材料科技股份有限公司 | Carbon crucible support and preparation method thereof |
| CN116003151A (en) * | 2022-07-18 | 2023-04-25 | 浙江星辉新材料科技有限公司 | A kind of carbon-carbon composite material crucible and preparation method thereof |
| CN116021802A (en) * | 2022-12-19 | 2023-04-28 | 贵州省紫安新材料科技有限公司 | Method for preparing heat-preserving barrel by short fiber mould pressing |
| CN116178036A (en) * | 2023-02-24 | 2023-05-30 | 陕西美兰德炭素有限责任公司 | Carbon-carbon composite material supporting rod and preparation method thereof |
| CN116947516A (en) * | 2023-07-27 | 2023-10-27 | 湖南湘投轻材科技股份有限公司 | Carbon fiber reinforced ceramic composite material and preparation method thereof |
| CN117658659A (en) * | 2023-11-11 | 2024-03-08 | 湖南碳谷新材料有限公司 | A single crystal furnace carbon energy-saving electrode and its preparation method |
| CN118184381A (en) * | 2024-03-13 | 2024-06-14 | 浙江星辉新材料科技有限公司 | Treatment method of carbon-carbon composite material waste |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114436670A (en) * | 2022-03-09 | 2022-05-06 | 西安美兰德新材料有限责任公司 | Winding forming-based high-strength carbon-carbon cylinder preparation method |
| CN116003151A (en) * | 2022-07-18 | 2023-04-25 | 浙江星辉新材料科技有限公司 | A kind of carbon-carbon composite material crucible and preparation method thereof |
| CN115231939A (en) * | 2022-07-22 | 2022-10-25 | 青岛晶易新材料科技股份有限公司 | Carbon crucible support and preparation method thereof |
| CN115231940A (en) * | 2022-08-01 | 2022-10-25 | 青岛晶易新材料科技股份有限公司 | Production process of carbon thermal insulation cylinder |
| CN116021802A (en) * | 2022-12-19 | 2023-04-28 | 贵州省紫安新材料科技有限公司 | Method for preparing heat-preserving barrel by short fiber mould pressing |
| CN116178036A (en) * | 2023-02-24 | 2023-05-30 | 陕西美兰德炭素有限责任公司 | Carbon-carbon composite material supporting rod and preparation method thereof |
| CN116178036B (en) * | 2023-02-24 | 2024-04-05 | 陕西美兰德新材料股份有限公司 | Carbon-carbon composite material supporting rod and preparation method thereof |
| CN116947516A (en) * | 2023-07-27 | 2023-10-27 | 湖南湘投轻材科技股份有限公司 | Carbon fiber reinforced ceramic composite material and preparation method thereof |
| CN117658659A (en) * | 2023-11-11 | 2024-03-08 | 湖南碳谷新材料有限公司 | A single crystal furnace carbon energy-saving electrode and its preparation method |
| CN118184381A (en) * | 2024-03-13 | 2024-06-14 | 浙江星辉新材料科技有限公司 | Treatment method of carbon-carbon composite material waste |
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Application publication date: 20211221 |
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