CN113024269A - Preparation method of high-performance super-large and super-thick carbon/carbon composite material - Google Patents
Preparation method of high-performance super-large and super-thick carbon/carbon composite material Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 59
- 239000002131 composite material Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 98
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 57
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 51
- 239000004917 carbon fiber Substances 0.000 claims abstract description 50
- 238000000034 method Methods 0.000 claims abstract description 43
- 238000005470 impregnation Methods 0.000 claims abstract description 24
- 238000003763 carbonization Methods 0.000 claims abstract description 22
- 238000003754 machining Methods 0.000 claims abstract description 14
- 238000005087 graphitization Methods 0.000 claims abstract description 12
- 238000000280 densification Methods 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims description 34
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- 239000007789 gas Substances 0.000 claims description 11
- 238000005229 chemical vapour deposition Methods 0.000 claims description 9
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 238000007598 dipping method Methods 0.000 claims description 6
- 239000007849 furan resin Substances 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 6
- 239000003345 natural gas Substances 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 3
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims description 3
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 3
- 238000012797 qualification Methods 0.000 abstract description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical group OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 9
- 239000000463 material Substances 0.000 description 7
- 238000012545 processing Methods 0.000 description 7
- 230000032798 delamination Effects 0.000 description 6
- 239000004744 fabric Substances 0.000 description 6
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 5
- 239000002699 waste material Substances 0.000 description 5
- 238000005336 cracking Methods 0.000 description 4
- 239000004952 Polyamide Substances 0.000 description 3
- 238000010000 carbonizing Methods 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 3
- 239000004745 nonwoven fabric Substances 0.000 description 3
- 229920002647 polyamide Polymers 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000036632 reaction speed Effects 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 230000008646 thermal stress Effects 0.000 description 2
- 238000002679 ablation Methods 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 150000001721 carbon Chemical class 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
The application provides a preparation method of a high-performance super-large and super-thick carbon/carbon composite material, which comprises the following steps: a. preparing a carbon fiber preform; b. carrying out primary graphitization treatment on the carbon fiber preform to obtain a carbon fiber blank; c. carrying out CVD densification treatment on the carbon fiber blank to obtain a CVD blank; d. carrying out secondary graphitization treatment on the CVD blank to obtain a graphitized blank; e. sequentially carrying out impregnation curing treatment, carbonization treatment, high-temperature heat treatment and machining treatment on the graphitized blank; f. repeating the step e until the density of the graphitized blank reaches a target value to obtain a primary finished product; g. and performing finish machining on the primary finished product to obtain a finished product. The product prepared by the method has high qualification rate and excellent performance, and can realize batch preparation of the high-performance super-large and super-thick carbon/carbon composite material.
Description
Technical Field
The invention relates to the technical field of composite material preparation and processing, in particular to a preparation method of a high-performance super-large and super-thick carbon/carbon composite material.
Background
The carbon/carbon composite material is a carbon matrix composite material reinforced by carbon fibers and fabrics thereof, has the advantages of low density, high strength, high specific modulus, high thermal conductivity, low expansion coefficient, good friction performance, good thermal shock resistance, high dimensional stability and the like, is a few of alternative materials applied at the temperature of more than 1650 ℃, has the highest theoretical temperature of 2600 ℃, is commonly used as a high-temperature ablation resistant material and a high-temperature structural material, has good application prospect in the fields of aviation, aerospace, nuclear energy, medicine, civil use and the like, and can be used for rocket and missile engine nozzles, aircraft antennas, airplanes, rail transit brake devices and other parts.
In the prior art, the carbon/carbon composite material is generally difficult to densify, and particularly, the process control difficulty is high during the production of the carbon/carbon composite material with the ultra-large and ultra-thick thickness (more than 1000mm multiplied by 300mm multiplied by 150 mm), the product quality and the performance are difficult to guarantee, and the related reports of the preparation of the high-performance ultra-large and ultra-thick carbon/carbon composite material are newly reported in the prior art.
Chinese patent CN109291544, a prefabricated structure of a carbon/carbon composite thick plate and a thick plate preparation method, the thickness of the prepared thick plate product is only 20-40 mm. In the process of mass production, the super-large and super-thick carbon/carbon composite material is easy to have quality problems of product deformation, delamination, cracks and the like during high-temperature heat treatment, the product percent of pass is not high, and the mechanical and thermal conductivity coefficients are low and the linear expansion coefficient is high.
Therefore, how to provide a method for preparing an ultra-large and ultra-thick carbon/carbon composite material with high product yield and excellent performance becomes a technical problem to be solved by technical personnel in the field.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of a high-performance super-large and super-thick carbon/carbon composite material, the product prepared by the method has high qualification rate and excellent performance, and the batch preparation of the high-performance super-large and super-thick carbon/carbon composite material can be realized.
The invention provides a preparation method of a high-performance super-large and super-thick carbon/carbon composite material, which comprises the following steps:
a. preparing a carbon fiber preform;
b. carrying out primary graphitization treatment on the carbon fiber preform to obtain a carbon fiber blank;
c. carrying out CVD densification treatment on the carbon fiber blank to obtain a CVD blank;
d. carrying out secondary graphitization treatment on the CVD blank to obtain a graphitized blank;
e. sequentially carrying out impregnation curing treatment, carbonization treatment, high-temperature heat treatment and machining treatment on the graphitized blank; the temperature rise process of the high-temperature heat treatment comprises the following steps: the room temperature is 1000 ℃ below zero, and the heating rate is 110-; 1500 ℃ at the temperature of 1000 ℃ and the heating rate of 90-140 ℃/h; 1500-; 1800 ℃ and 2200 ℃, and the heating rate is 60-110 ℃/h; 2200- (2300) and 2600 ℃, the heating rate is 45-90 ℃/h, 2300 and 2600 ℃, and the temperature is kept for 2-5 h.
The machining process comprises the steps of removing a surface compact layer with a preset thickness;
f. repeating the step e until the density of the graphitized blank reaches a target value to obtain a primary finished product;
g. and performing finish machining on the primary finished product to obtain a finished product.
In the present invention, the high-temperature heat treatment is performed to convert the structure of the carbon material. Because the blank has large and thick size, the reaction speed of the internal structure conversion of the material is slowed down in order to avoid the delamination, deformation and cracking of the blank, the high-temperature heat treatment is carried out in a step heating mode, and the heating rate is determined according to the intensity of the carbon structure conversion reaction speed.
Furthermore, in the step e, in the cooling stage of the high-temperature heat treatment, since the blank is large and thick, in order to avoid the delamination, deformation and cracking of the blank and slow down the release of the thermal stress in the material, the cooling stage is performed in a stepped cooling manner.
Preferably, the cooling process of the high-temperature heat treatment is as follows: (2600-; 2200 ℃ and 1800 ℃, and the cooling rate is 60-90 ℃/h; 1800 plus temperature at 1000 ℃, and the cooling rate is 70-110 ℃/h; 1000 ℃ to room temperature, and naturally cooling along with the furnace.
The stepped cooling is beneficial to avoiding the concentration of thermal stress in a high-temperature environment and avoiding the deformation, delamination and cracking of the blank.
Preferably, the preset thickness is 0.5-2 mm.
Preferably, the preset thickness is 1 mm.
Preferably, the target value is not less than 1.85g/cm3. Preferably, the process parameters of the CVD densification treatment are as follows: the carbon source gas is natural gas or propylene, the furnace temperature is 950-1120 ℃, the furnace pressure is 3-15kPa, and the chemical vapor deposition time is 200-400 h.
In the step e, the carbonization treatment is used for slowly removing most non-carbon substances in the resin, so that the blank is prevented from being over-excited during high-temperature heat treatment. In the invention, the blank is large and thick, so that in order to avoid the delamination and deformation of the blank, the carbonization treatment is carried out in a step heating mode, and the heating rate is determined according to the reaction severity of the resin in each temperature interval.
Preferably, the temperature rise process of the carbonization treatment is as follows: the room temperature is 200 ℃ below zero, and the heating rate is 40-60 ℃/h; 200 and 350 ℃, and the heating rate is 20-40 ℃/h; 350-500 ℃, and the heating rate is 10-20 ℃/h; 500 ℃ and 700 ℃, the heating rate is 20-40 ℃/h; 700- (1000-1200) DEG C, the heating rate is 40-55 ℃/h; (1000-.
Preferably, the technological parameters of the dipping and curing treatment are as follows: the impregnation liquid is furan resin, 3-10% of curing agent is added, the impregnation time is 2-5h, the curing temperature is 160-220 ℃, and the curing and heat preservation time is 2-5 h.
Specifically, the curing agent is phosphoric acid.
Preferably, the technological parameters of the dipping and curing treatment are as follows: the impregnation liquid is furan resin, 6% phosphoric acid is added as a curing agent, the impregnation time is 3h, the curing temperature is 160 ℃, and the curing and heat preservation time is 3 h.
Preferably, the step b specifically comprises: and putting the carbon fiber preform into a heat treatment furnace, vacuumizing, heating to 2000-2500 ℃, preserving heat for 1-3h, introducing argon gas during the period, keeping the furnace pressure at 0.2-3KPa, graphitizing the carbon fiber preform, and naturally cooling to obtain a carbon fiber blank.
Preferably, the step d specifically comprises: putting the CVD blank into a heat treatment furnace, firstly vacuumizing, heating to 2000-2500 ℃, then preserving heat for 1-3h, introducing argon gas during the period, and keeping the furnace pressure at 0.2-3KPa to graphitize the CVD blank, and naturally cooling to obtain the graphitized blank.
Preferably, the density of the carbon fiber preform is 0.3 to 0.6g/cm3。
Preferably, the carbon fiber preform is of a 2D needling structure, and one layer of PANCF weftless fabric mesh tire are alternately layered.
Preferably, the non-woven fabric is formed by continuously needling 0 DEG/90 DEG alternately laid layers.
Preferably, the size of the carbon fiber preform is 5-20mm larger than the size of the finished product.
The invention has the following beneficial effects:
(1) according to the preparation method of the high-performance ultra-large and ultra-thick carbon/carbon composite material, a mode of step temperature rise and drop is adopted in the high-temperature heat treatment process, the problems that a blank is easy to layer, deform, crack and the like in the production process of the ultra-large and ultra-thick carbon/carbon composite material are effectively solved, and the high-temperature heat treatment period is shortened; the super-large and super-thick carbon/carbon composite material prepared by the method has the advantages of high product qualification rate, excellent mechanical property index, high heat conductivity coefficient and low linear expansion coefficient.
(2) The carbon/carbon composite material with large size and thickness prepared by the method provided by the invention has the length of more than 1300mm, the width of more than 300mm and the thickness of more than 150 mm;
the performance index can reach: the density is more than or equal to 1.85g/cm3The compressive strength is more than or equal to 265MPa, the tensile strength is more than or equal to 170MPa, the bending strength is more than or equal to 175MPa, and the interlaminar shear strength is more than or equal to 85MPa, so that the material has good material performance and development and application prospects.
Drawings
FIG. 1 is a schematic structural view of a finished product in example 1;
FIG. 2 is a schematic structural view of a finished product in comparative example 2;
fig. 3 is a schematic structural view of the finished product in comparative example 3.
Detailed Description
In order to make those skilled in the art better understand the technical solutions in the present application, the present application will be clearly and completely described below with reference to specific embodiments, and it is obvious that the described embodiments are only a part of the embodiments of the present application, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
Example 1
a. Preparing 15 carbon fiber preforms, wherein the carbon fiber preforms are of a 2D needling structure, and are formed by adopting a layer of PANCF (polyamide fiber reinforced fabric) laid layer and a layer of PANCF mesh tire alternately, laying the layers of the non-woven fabric alternately at an angle of 0 degree/90 degree and continuously needling; the carbon fiber preform has dimensions of 1370mm × 390mm × 190mm and a density of 0.58g/cm3;
b. Carrying out primary graphitization treatment on the carbon fiber preform to obtain a carbon fiber blank; putting the carbon fiber preform into a heat treatment furnace, vacuumizing, heating to 2000 ℃, preserving heat for 2 hours, introducing argon gas during the period, and keeping the furnace pressure at 0.2-3KPa to graphitize the carbon fiber preform, and then naturally cooling along with the furnace;
c. carrying out CVD densification treatment on the carbon fiber blank, loading the carbon fiber blank into a chemical vapor deposition furnace, carrying out chemical vapor deposition at 1070 ℃ by using natural gas as a carbon source gas for 350h, wherein the furnace pressure is 5-15kPa, and the blank density reaches 1.35g/cm3Obtaining a CVD blank;
d. carrying out secondary graphitization treatment on the CVD blank to obtain a graphitized blank;
e. sequentially carrying out impregnation curing treatment, carbonization treatment, high-temperature heat treatment and machining treatment on the graphitized blank;
the impregnation curing treatment adopts furan resin, 5 percent phosphoric acid is added as a curing agent, an impregnation tank is vacuumized and then is filled with nitrogen to 2MPa, the impregnation time is 2 hours, the curing temperature is 200 ℃, and the curing and heat preservation time is 2 hours;
carbonizing the blank subjected to the dipping and curing treatment in a carbonization furnace, wherein the atmosphere in the furnace is nitrogen, and the furnace pressure is 0-5 Kpa; the step heating process in the carbonization process comprises the following steps: the room temperature is 200 ℃ below zero, and the heating rate is 50 ℃/h; 200 and 350 ℃, and the heating rate is 20 ℃/h; 350-500 ℃, and the heating rate is 15 ℃/h; 500 ℃ and 700 ℃, and the heating rate is 20 ℃/h; 700 ℃ and 1000 ℃, and the heating rate is 30 ℃/h; preserving heat for 3 hours at 1000 ℃;
the step heating process of the high-temperature heat treatment comprises the following steps: the room temperature is 1000 ℃ below zero, and the heating rate is 130 ℃/h; 1000 and 1500 ℃, and the heating rate is 105 ℃/h; 1500-; 1800 ℃ and 2200 ℃, and the heating rate is 70 ℃/h; 2200 ℃ and 2400 ℃ and the heating rate is 55 ℃/h; keeping the temperature at 2400 ℃ for 4 h;
the step cooling process of the high-temperature heat treatment comprises the following steps: 2400 ℃ and 2200 ℃, and the cooling rate is 60 ℃/h; 2200 ℃ and 1800 ℃ with the cooling rate of 65 ℃/h; 1800 plus temperature at 1000 ℃, and the cooling rate at 80 ℃/h; cooling naturally with the furnace at 1000-room temperature;
after high-temperature heat treatment, carrying out mechanical processing treatment on the surface of the blank to remove a surface compact layer with a preset thickness, wherein the preset thickness is 1 mm;
f. the above operations of 'impregnation curing treatment-carbonization treatment-high temperature heat treatment-mechanical processing' are circularly carried out for 9 times, so that the density of the blank body reaches 1.85g/cm3Obtaining a primary finished product;
g. performing finish machining on the primary finished product to obtain a finished product; the product size is 1355mm multiplied by 375mm multiplied by 175mm, wherein 2 products are deformed waste products, the product percent of pass reaches 86.7%, and the product performance index data is shown in table 1.
Example 2
a. Preparing 35 carbon fiber preforms, wherein the carbon fiber preforms are of a 2D needling structure, and are formed by adopting a layer of PANCF (polyamide fiber reinforced fabric) laid layer and a layer of PANCF mesh tire alternately, laying the laid cloth at 0 degree/90 degree alternately and continuously needling; the carbon fiber preform had dimensions of 1240 mm. times.340 mm. times.170 mm and a density of 0.45g/cm3;
b. Carrying out primary graphitization treatment on the carbon fiber preform to obtain a carbon fiber blank; putting the carbon fiber preform into a heat treatment furnace, vacuumizing, heating to 2000 ℃, preserving heat for 2 hours, introducing argon gas during the period, and keeping the furnace pressure at 0.2-3KPa to graphitize the carbon fiber preform, and then naturally cooling along with the furnace;
c. carrying out CVD densification treatment on the carbon fiber blank, loading the carbon fiber blank into a chemical vapor deposition furnace, carrying out chemical vapor deposition at 1000 ℃ by using propylene as a carbon source gas, wherein the deposition time is 300h, the furnace pressure is 3-8kPa, and the blank density reaches 1.42g/cm3And obtaining a CVD blank.
d. Carrying out secondary graphitization treatment on the CVD blank to obtain a graphitized blank;
e. sequentially carrying out impregnation curing treatment, carbonization treatment, high-temperature heat treatment and machining treatment on the graphitized blank;
the impregnation curing treatment adopts furan resin, 6 percent phosphoric acid is added as a curing agent, an impregnation tank is vacuumized and then is filled with nitrogen to 3MPa, the impregnation time is 3 hours, the curing temperature is 160 ℃, and the curing and heat preservation time is 3 hours;
carbonizing the blank subjected to the dipping and curing treatment in a carbonization furnace, wherein the atmosphere in the furnace is nitrogen, and the furnace pressure is 0-5 Kpa; the step heating process in the carbonization process comprises the following steps: the room temperature is 200 ℃ below zero, and the heating rate is 55 ℃/h; 200 and 350 ℃, and the heating rate is 25 ℃/h; 350-500 ℃, and the heating rate is 20 ℃/h; 500 ℃ and 700 ℃, the heating rate is 25 ℃/h; 700 ℃ and 1000 ℃, and the heating rate is 35 ℃/h; preserving heat for 3 hours at 1000 ℃;
the step heating process of the high-temperature heat treatment comprises the following steps: the room temperature is 1000 ℃ below zero, and the heating rate is 135 ℃/h; 1000 and 1500 ℃, and the heating rate is 110 ℃/h; 1500-; 1800 ℃ and 2200 ℃ with the heating rate of 75 ℃/h; 2200 ℃ and 2400 ℃ and the heating rate is 60 ℃/h; keeping the temperature at 2400 ℃ for 3 h;
the step cooling process of the high-temperature heat treatment comprises the following steps: 2400 ℃ and 2200 ℃, and the cooling rate is 65 ℃/h; 2200 ℃ and 1800 ℃, and the cooling rate is 70 ℃/h; 1800 plus temperature at 1000 ℃, and the cooling rate at 85 ℃/h; cooling naturally with the furnace at 1000-room temperature;
after high-temperature heat treatment, carrying out mechanical processing treatment on the surface of the blank to remove a surface compact layer with a preset thickness, wherein the preset thickness is 1 mm;
f. the above operations of 'impregnation curing treatment-carbonization treatment-high temperature heat treatment-mechanical processing' are circularly carried out for 9 times, so that the density of the blank body reaches 1.85g/cm3Obtaining a primary finished product;
g. performing finish machining on the primary finished product to obtain a finished product; the product size is 1225mm multiplied by 325mm multiplied by 155mm, wherein 3 products are layered waste products, the product percent of pass reaches 92.5%, and the product performance index data is shown in table 1.
Example 3
a. Preparing 50 carbon fiber preforms, wherein the carbon fiber preforms are of a 2D needling structure, and are formed by adopting a layer of PANCF (polyamide fiber fabric) laid alternately with a layer of PANCF mesh tire, laying the layers of the non-woven fabric alternately at an angle of 0 DEG/90 DEG and continuously needling; the size of the carbon fiber preform is 1015mm multiplied by 315mm multiplied by 165mm, and the felt bulk density is 0.35g/cm3;
b. Carrying out primary graphitization treatment on the carbon fiber preform to obtain a carbon fiber blank; putting the carbon fiber preform into a heat treatment furnace, vacuumizing, heating to 2000 ℃, preserving heat for 2 hours, introducing argon gas during the period, and keeping the furnace pressure at 0.2-3KPa to graphitize the carbon fiber preform, and then naturally cooling along with the furnace;
c. carrying out CVD densification treatment on the carbon fiber blank, loading the carbon fiber blank into a chemical vapor deposition furnace, carrying out chemical vapor deposition at 1100 ℃ by using natural gas as a carbon source gas for 200h, wherein the furnace pressure is less than or equal to 5-15kPa, and the blank density reaches 1.51g/cm3Obtaining a CVD blank;
d. carrying out secondary graphitization treatment on the CVD blank to obtain a graphitized blank;
e. sequentially carrying out impregnation curing treatment, carbonization treatment, high-temperature heat treatment and machining treatment on the graphitized blank;
the impregnation curing treatment adopts furan resin, 7 percent phosphoric acid is added as a curing agent, an impregnation tank is vacuumized and then is filled with nitrogen to 3MPa, the impregnation time is 3 hours, the curing temperature is 160 ℃, and the curing and heat preservation time is 3 hours;
carbonizing the blank subjected to the dipping and curing treatment in a carbonization furnace, wherein the atmosphere in the furnace is nitrogen, and the furnace pressure is 0-5 Kpa; the step heating process in the carbonization process comprises the following steps: the room temperature is 200 ℃ below zero, and the heating rate is 60 ℃/h; 200 and 350 ℃, and the heating rate is 30 ℃/h; 350-500 ℃, and the heating rate is 25 ℃/h; 500 ℃ and 700 ℃, the heating rate is 30 ℃/h; 700 ℃ and 1000 ℃, the heating rate is 40 ℃/h; preserving heat for 2 hours at 1000 ℃;
the step heating process of the high-temperature heat treatment comprises the following steps: the room temperature is 1000 ℃, and the heating rate is 140 ℃/h; 1000-; 1500-; 1800 ℃ and 2200 ℃, and the heating rate is 80 ℃/h; 2200 ℃ and 2400 ℃ and the heating rate is 65 ℃/h; keeping the temperature at 2400 ℃ for 2 h;
the step cooling process of the high-temperature heat treatment comprises the following steps: 2400 ℃ and 2200 ℃, and the cooling rate is 70 ℃/h; 2200 ℃ and 1800 ℃ with the cooling rate of 75 ℃/h; 1800 plus temperature at 1000 ℃, and the cooling rate at 90 ℃/h; cooling naturally with the furnace at 1000-room temperature;
after high-temperature heat treatment, carrying out mechanical processing treatment on the surface of the blank to remove a surface compact layer with a preset thickness, wherein the preset thickness is 1 mm;
f. the above operations of 'impregnation curing treatment-carbonization treatment-high temperature heat treatment-mechanical processing' are circularly carried out for 9 times, so that the density of the blank body reaches 1.85g/cm3Obtaining a primary finished product;
g. performing finish machining on the primary finished product to obtain a finished product; the product size is 1000mm multiplied by 300mm multiplied by 150mm, no layering, cracks and deformation waste products appear, the qualification rate reaches 100%, and the product performance index data is shown in table 1.
Comparative example 1
Compared with the example 1, the other treatment processes and the process parameters are the same, only the chemical vapor deposition process is not carried out, 20 products are produced, 3 products are cracked, the product percent of pass is 85%, and the physical and mechanical properties (shown in the table 1) of the products are about 40% lower than those of the example 1.
Comparative example 2
Compared with the embodiment 1, other treatment processes and process parameters are the same, and only a step heating process is not adopted during carbonization treatment, but the temperature is raised to 1000 ℃ at one time and is kept for 3 hours; the high-temperature heat treatment does not adopt a step heating and cooling process, but once heats up to 2400 ℃ and preserves the temperature for 4 hours, then cools down to 1000 ℃, and then naturally cools down to room temperature along with the furnace.
10 products are produced in the comparative example 2, 5 of the products are deformed, layered and cracked waste products, the yield is 50%, and the performance index data of the products are shown in the table 1.
Comparative example 3
Compared with the embodiment 2, other treatment processes and process parameters are the same, the carbonization treatment process and the high-temperature heat treatment process are carried out in a step temperature rise mode, but the high-temperature heat treatment process does not adopt a step temperature reduction process, and the carbonization treatment process and the high-temperature heat treatment process are naturally cooled to room temperature along with the furnace after being cooled to 1000 ℃.
In comparative example 3, 20 products were produced, 6 of the products were waste products of deformation, delamination and cracking, the percent of pass was 70%, and the product performance index data are shown in table 1.
TABLE 1 product Performance index data Table for examples 1-3 and comparative examples 1-3
As can be seen from the data in Table 1, the product properties produced by examples 1-3 are much higher than those of comparative examples 1-3; and the product yield in examples 1-3 is much higher than in comparative examples 1-3.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. A preparation method of a high-performance super-large and super-thick carbon/carbon composite material is characterized by comprising the following steps:
a. preparing a carbon fiber preform;
b. carrying out primary graphitization treatment on the carbon fiber preform to obtain a carbon fiber blank;
c. carrying out CVD densification treatment on the carbon fiber blank to obtain a CVD blank;
d. carrying out secondary graphitization treatment on the CVD blank to obtain a graphitized blank;
e. sequentially carrying out impregnation curing treatment, carbonization treatment, high-temperature heat treatment and machining treatment on the graphitized blank;
the temperature rise process of the high-temperature heat treatment comprises the following steps: the room temperature is 1000 ℃ below zero, and the heating rate is 110-; 1500 ℃ at the temperature of 1000 ℃ and the heating rate of 90-140 ℃/h; 1500-; 1800 ℃ and 2200 ℃, and the heating rate is 60-110 ℃/h; 2200- (2300) and 2600 ℃, the heating rate is 45-90 ℃/h, 2300 and 2600 ℃, and the temperature is kept for 2-5 h.
The machining process comprises the steps of removing a surface compact layer with a preset thickness;
f. repeating the step e until the density of the graphitized blank reaches a target value to obtain a primary finished product;
g. and performing finish machining on the primary finished product to obtain a finished product.
2. The method for preparing the high-performance ultra-large and ultra-thick carbon/carbon composite material according to claim 1, wherein the cooling process of the high-temperature heat treatment comprises the following steps: (2600-; 2200 ℃ and 1800 ℃, and the cooling rate is 60-90 ℃/h; 1800 plus temperature at 1000 ℃, and the cooling rate is 70-110 ℃/h; 1000 ℃ to room temperature, and naturally cooling along with the furnace.
3. The method of claim 1, wherein the predetermined thickness is 0.5-2 mm.
4. The method of claim 3, wherein the predetermined thickness is 1 mm.
5. The method of claim 1, wherein the carbon/carbon composite is prepared by a process comprising the steps ofThe target value is more than or equal to 1.85g/cm3。
6. The method for preparing the high-performance ultra-thick carbon/carbon composite material according to claim 1, wherein the CVD densification treatment comprises the following process parameters:
the carbon source gas is natural gas or propylene, the furnace temperature is 950-1120 ℃, the furnace pressure is 3-15kPa, and the chemical vapor deposition time is 200-400 h.
7. The preparation method of the high-performance extra-large and extra-thick carbon/carbon composite material according to claim 1, wherein the temperature rise process of the carbonization treatment comprises the following steps: the room temperature is 200 ℃ below zero, and the heating rate is 40-60 ℃/h; 200 and 350 ℃, and the heating rate is 20-40 ℃/h; 350-500 ℃, and the heating rate is 10-20 ℃/h; 500 ℃ and 700 ℃, the heating rate is 20-40 ℃/h; 700- (1000-1200) DEG C, the heating rate is 40-55 ℃/h; (1000-.
8. The method for preparing the high-performance extra-large and extra-thick carbon/carbon composite material according to claim 1, wherein the technological parameters of the dipping and curing treatment are as follows: the impregnation liquid is furan resin, 3-10% of curing agent is added, the impregnation time is 2-5h, the curing temperature is 160-220 ℃, and the curing and heat preservation time is 2-5 h.
9. The method for preparing a high-performance extra-large and extra-thick carbon/carbon composite material according to claim 1, wherein the step b specifically comprises the following steps: and putting the carbon fiber preform into a heat treatment furnace, vacuumizing, heating to 2000-2500 ℃, preserving heat for 1-3h, introducing argon gas during the period, keeping the furnace pressure at 0.2-3KPa, graphitizing the carbon fiber preform, and naturally cooling to obtain a carbon fiber blank.
10. The method of claim 1, wherein the carbon fiber preform has a density of 0.3-0.6g/cm3。
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
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Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2000103686A (en) * | 1998-09-29 | 2000-04-11 | Tokai Carbon Co Ltd | Production of carbon fiber reinforced carbon composite material |
CN102167611A (en) * | 2011-01-27 | 2011-08-31 | 无锡市弟兆碳材料有限公司 | Method for preparing carbon/carbon composite material plate |
CN103387406A (en) * | 2013-07-10 | 2013-11-13 | 航天材料及工艺研究所 | Preparation method of dimensional and high thermal conductivity carbon/carbon compound material |
CN105801146A (en) * | 2016-04-15 | 2016-07-27 | 航天材料及工艺研究所 | Continuous density gradient low-density porous carbon bonding composite material and preparing method thereof |
CN111635242A (en) * | 2020-06-09 | 2020-09-08 | 中南大学 | Rapid preparation method and application of high-density revolving body carbon/carbon composite material |
CN111825473A (en) * | 2020-07-29 | 2020-10-27 | 湖南博云新材料股份有限公司 | Preparation method of carbon/carbon composite material |
-
2021
- 2021-03-19 CN CN202110297552.3A patent/CN113024269A/en active Pending
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2000103686A (en) * | 1998-09-29 | 2000-04-11 | Tokai Carbon Co Ltd | Production of carbon fiber reinforced carbon composite material |
CN102167611A (en) * | 2011-01-27 | 2011-08-31 | 无锡市弟兆碳材料有限公司 | Method for preparing carbon/carbon composite material plate |
CN103387406A (en) * | 2013-07-10 | 2013-11-13 | 航天材料及工艺研究所 | Preparation method of dimensional and high thermal conductivity carbon/carbon compound material |
CN105801146A (en) * | 2016-04-15 | 2016-07-27 | 航天材料及工艺研究所 | Continuous density gradient low-density porous carbon bonding composite material and preparing method thereof |
CN111635242A (en) * | 2020-06-09 | 2020-09-08 | 中南大学 | Rapid preparation method and application of high-density revolving body carbon/carbon composite material |
CN111825473A (en) * | 2020-07-29 | 2020-10-27 | 湖南博云新材料股份有限公司 | Preparation method of carbon/carbon composite material |
Cited By (12)
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---|---|---|---|---|
CN115385709A (en) * | 2022-08-23 | 2022-11-25 | 湖南博云新材料股份有限公司 | Method for quickly compacting carbon-carbon composite material |
CN115385709B (en) * | 2022-08-23 | 2023-09-29 | 湖南博云新材料股份有限公司 | Method for quickly compacting carbon-carbon composite material |
CN115894080A (en) * | 2022-09-09 | 2023-04-04 | 湖南博云新材料股份有限公司 | Method for preparing antioxidant coating on graphite surface |
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CN115448744A (en) * | 2022-09-14 | 2022-12-09 | 湖南博云新材料股份有限公司 | Preparation method of carbon/carbon throat insert |
CN115448744B (en) * | 2022-09-14 | 2023-09-12 | 湖南博云新材料股份有限公司 | Preparation method of carbon/carbon throat liner |
CN115872766A (en) * | 2022-11-14 | 2023-03-31 | 湖南碳谷新材料有限公司 | Preparation method of carbon-carbon material heat preservation device and heat preservation device |
CN115872766B (en) * | 2022-11-14 | 2024-01-02 | 湖南碳谷新材料有限公司 | Preparation method of carbon-carbon material heat preservation device and heat preservation device |
CN115745646A (en) * | 2022-11-28 | 2023-03-07 | 湖南博云新材料股份有限公司 | Preparation method of carbon/carbon composite material |
CN115745646B (en) * | 2022-11-28 | 2024-03-08 | 湖南博云新材料股份有限公司 | Preparation method of carbon/carbon composite material |
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