CN113248275B - Light carbon fiber/carbon cylinder thermal field material with graphite coating coated on surface and preparation method thereof - Google Patents

Light carbon fiber/carbon cylinder thermal field material with graphite coating coated on surface and preparation method thereof Download PDF

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CN113248275B
CN113248275B CN202110753363.2A CN202110753363A CN113248275B CN 113248275 B CN113248275 B CN 113248275B CN 202110753363 A CN202110753363 A CN 202110753363A CN 113248275 B CN113248275 B CN 113248275B
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carbon fiber
carbon
thermal field
light
graphite coating
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CN113248275A (en
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唐波
吴新锋
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Hangzhou Vulcan New Material Technology Co ltd
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Hangzhou Vulcan New Material Technology Co ltd
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Abstract

The invention provides a light carbon fiber/carbon cylinder thermal field material with a graphite coating coated on the surface and a preparation method thereof. The invention uses ultraviolet light to initiate vinyl crosslinking reaction, then initiates phenol furfural polycondensation reaction to form phenol furfural crosslinking network through heat released in the process of photo-initiation vinyl crosslinking reaction, multiple network cured products are quickly prepared into a light carbon fiber/carbon cylinder thermal field material blank through high-temperature carbonization and graphitization, and the obtained light carbon fiber/carbon cylinder thermal field material blank is processed, sprayed with a graphite coating on the surface and purified by high-temperature and chemical gas to prepare the light carbon fiber/carbon cylinder thermal field material with low density, excellent mechanical property, good thermal insulation property and high purity and coated with the graphite coating on the surface. The performance of the obtained light carbon fiber/carbon cylinder thermal field material with the graphite coating coated on the surface can reach the following indexes: the bending strength is 3.5MPa, and the density can be controlled at 0.15g/cm3The impurity content is 5ppm, and the thermal conductivity is 0.15W/(mK).

Description

Light carbon fiber/carbon cylinder thermal field material with graphite coating coated on surface and preparation method thereof
Technical Field
The invention relates to the technical field of carbon fiber/carbon composite cylindrical thermal field materials, in particular to a light carbon fiber/carbon cylindrical thermal field material with a graphite coating coated on the surface and a preparation method thereof.
Background
The light carbon fiber/carbon cylinder thermal field material has the advantages of low overall density, good thermal field heat preservation performance, low metal impurity content, namely high purity and the like, and is widely applied to high-temperature thermal fields such as a monocrystalline silicon czochralski furnace thermal field, a silicon semiconductor crystal growth furnace thermal field, a silicon carbide semiconductor crystal growth furnace thermal field, an optical fiber drawing furnace thermal field, a sapphire crystal growth furnace thermal field and the like.
However, in the preparation process of the existing carbon fiber/carbon cylinder thermal field material, the main preparation process comprises the following steps: cutting a carbon fiber soft felt, impregnating phenolic resin, winding and curing, carbonizing at high temperature and graphitizing, and processing. The preparation process has the following problems: (1) in the impregnation process, solvents such as alcohol and the like are added to reduce the viscosity of the resin in the process of impregnating the carbon fiber soft felt with the phenolic resin, so that the carbon fiber soft felt and the phenolic resin are fully impregnated, the impregnation uniformity is improved, then the treatment is carried out in a drying mode, and the addition of the solvents can cause environmental pollution; (2) in the winding and curing process, the phenolic resin in the carbon fiber felt impregnated with the phenolic resin is easy to generate glue flowing phenomenon in the curing process due to the action of gravity, so that the resin impregnation is not uniform, in addition, the whole curing process takes more than 10 hours, the production efficiency is low, and meanwhile, a large amount of energy consumption is consumed for heating by a press; (4) in the high-temperature carbonization and graphitization processes, the arc-shaped structure of the carbon fiber felt enables the carbon fiber felt to have stress concentration and easily deform; (5) a large number of pores exist on the surface of the processed carbon fiber/carbon cylinder thermal field material, so that the thermal insulation performance of the material is poor.
The problems of solvent volatilization, environmental pollution, curing gummosis, uneven dipping, high curing energy consumption, low efficiency, stress deformation, poor heat preservation and the like are urgently needed to be solved by a new material and a new method.
Disclosure of Invention
The invention aims to overcome the defects of the existing material and the preparation method and provide the light carbon fiber/carbon cylinder thermal field material with the graphite coating coated on the surface, which has the advantages of small density, good heat insulation performance, high purity, high strength, simple and quick preparation process.
The invention also aims to provide a method for preparing the light carbon fiber/carbon cylinder thermal field material with the graphite coating coated on the surface, which has a novel resin structure and is rapid in curing and forming.
The invention uses ultraviolet light to initiate vinyl crosslinking reaction, then initiates phenol furfural polycondensation reaction to form phenol furfural crosslinking network through heat released in the process of photo-initiation vinyl crosslinking reaction, multiple network cured products are quickly prepared into a light carbon fiber/carbon cylinder thermal field material blank through high-temperature carbonization and graphitization, and the obtained light carbon fiber/carbon cylinder thermal field material blank is processed, sprayed with a graphite coating on the surface and purified by high-temperature and chemical gas to prepare the light carbon fiber/carbon cylinder thermal field material with low density, excellent mechanical property, good thermal insulation property and high purity and coated with the graphite coating on the surface.
The technical scheme adopted by the invention is as follows:
the light carbon fiber/carbon cylinder thermal field material with the graphite coating coated on the surface comprises the following raw materials in parts by weight:
carbon fiber soft felt: 100 portions of
Phenol: 10-30 parts of
And (3) furfural: 8 to 24 portions of
Ammonia water: 0.4 to 1.2 portions of
Vinyl co-crosslinking agent: 1-3 parts of
Photoinitiator (2): 0.1 to 0.3 portion
The carbon fiber soft felt is prepared from long carbon fibers through an air-laid and needle-punched felt forming process, and the ratio of Z-direction fibers to X-Y in-plane fibers of the activated carbon fiber soft felt is 1: (50-150) the density is 500-700 g/cm2The thickness is 10 +/-1 mm; the length of the long carbon fiber is 10-15 cm.
And performing condensation reaction on the furfural and phenol under the catalysis of crosslinking heat and ammonia water to form a furfural-phenol resin crosslinked network.
The mass concentration of the ammonia water is 10-100%.
The ammonia water initiates phenol and furfural to carry out polycondensation reaction under the action of double bond crosslinking heat, and plays a role of an initiator.
The vinyl auxiliary crosslinking agent includes but is not limited to vinyl bond-containing monovinyl low molecular compound, divinyl crosslinking agent and polyvinyl crosslinking agent;
wherein, the monoethylene low molecular compound includes but is not limited to styrene, acrylate; divinyl crosslinkers include, but are not limited to, tripropylene glycol dipropylene ether ester; polyvinyl crosslinkers include, but are not limited to, trimethylolpropane triacrylate, trimethylolpropane trimethacrylate, triallyl isocyanurate;
when the vinyl auxiliary crosslinking agent is an acrylic compound, the vinyl auxiliary crosslinking agent can play a role in promoting crosslinking, and can perform a co-crosslinking reaction with double bonds on furfural under the decomposition of an initiator initiated by ultraviolet light or under the action of excited energy to form a photoinitiated vinyl crosslinking network. The photoinitiated vinyl crosslinked network further forms a cross network with the phenol furfural resin condensation crosslinked network, so that the distance between benzene ring structures in the whole large crosslinked network is shortened, high carbon residue is formed in the high-temperature carbonization and graphitization processes, and the strength of the carbon fiber/carbon material is improved.
The photoinitiator is a free radical photoinitiator or a cationic photoinitiator. Wherein the free radical photoinitiator includes, but is not limited to, benzoin butyl ether, benzoin dimethyl ether, benzoin ethyl ether, benzoin isopropyl ether, alpha-dimethoxy-alpha-phenylacetophenone, diphenylethanone, alpha-hydroxyalkylphenone, alpha-aminoalkylphenone, alpha-diethoxyacetophenone, bisbenzoylphenylphosphine oxide, aroylphosphine oxide, 2, 4-dihydroxybenzophenone, benzophenone, thiopropoxythioxanthone, isopropyl thioxanthone; the cationic photoinitiator includes, but is not limited to, diaryliodonium salts, triaryliodonium salts, alkyl iodonium salts, cumeneferrocene hexafluorophosphate.
Wherein, the photoinitiator is decomposed or in an excited state under the irradiation of ultraviolet light, the double bond on the furfural and the double bond on the vinyl crosslinking agent are initiated to carry out crosslinking reaction, heat is released, and then the condensation reaction of phenol and furfural is further initiated.
A light carbon fiber/carbon cylinder thermal field material with a graphite coating coated on the surface comprises the following raw materials in parts by weight:
graphite flake: 100 portions of
Polyvinyl butyral: 10-30 parts of
Phenolic resin aqueous solution: 200 portions and 600 portions
The graphite sheet is 30-80um in size and about 10um in thickness.
The polyvinyl butyral is chemically pure, and a graphite sheet can be adhered to the surface of the light carbon fiber/carbon thermal field blank material.
The phenolic resin aqueous solution is a mixture of water-soluble phenolic resin and water, wherein the solid content is 40-75%, and the phenolic resin aqueous solution plays a role in adhering the graphite sheet with the high-temperature residual carbon.
After the surface graphite coating material is coated on the surface of the light carbon fiber/carbon thermal field blank material, the blank material is placed at normal temperature for 0.5 to 3 hours, and then the blank material can be placed into a purifying furnace for high-temperature purification treatment.
The invention also aims to provide a method for preparing the light carbon fiber/carbon cylinder thermal field material with the graphite coating coated on the surface, which has high production efficiency, low energy consumption, little pollution, high purity and good heat-insulating property, namely, high efficiency and low energy consumption.
A preparation method of a light carbon fiber/carbon cylinder thermal field material with a graphite coating coated on the surface comprises the following steps:
(1) spraying glue, dipping, curing and forming: (a) resin impregnation: winding the carbon fiber soft felt on a cylindrical metal die, and then directly spraying and impregnating a resin system of phenol, a vinyl auxiliary crosslinking agent, furfural, ammonia water and a photoinitiator with the carbon fiber soft felt; (b) ultraviolet light initiated double bond reaction: exciting a photoinitiator by ultraviolet light to enable the initiator to be in a free radical state or an excited state, then initiating a vinyl crosslinking reaction between the furfural resin and the vinyl co-crosslinking agent to form a vinyl crosslinking network, and simultaneously releasing a large amount of reaction heat; (c) phenol furfural condensation reaction: the vinyl crosslinking reaction heat promotes ammonia water to initiate phenol furfural polycondensation crosslinking reaction of furfural and phenol compounds to form a phenolic crosslinking network, and the vinyl crosslinking network and the phenolic crosslinking network are crossed with each other to form a double-crosslinking cured product.
(2) Carbonization and graphitization: and removing the metal mould from the carbon fiber felt curing product, mounting a carbon/carbon mould, binding a carbon fiber rope on the outer surface, directly performing carbonization and graphitization reaction in a high-temperature furnace, and quickly preparing the light carbon fiber/carbon cylinder composite thermal field blank material.
(3) Graphitizing the coating: the light carbon fiber/carbon cylinder composite thermal field blank material is processed to the required size, and then the surface graphite coating system material is sprayed by a spray gun.
(4) And (3) purification: and (3) putting the carbon fiber/carbon cylinder thermal field material coated with the graphitized coating into a purification furnace for purification treatment, and discharging to obtain the light carbon fiber/carbon cylinder thermal field material coated with the graphite coating on the surface.
In the step (1), the carbon fiber soft felt is directly sprayed and liquid-phase impregnated, so that the resin is fully contacted with the carbon fiber soft felt, and the carbon fiber is impregnated by using the low-viscosity polymer precursor, so that the impregnation efficiency is high.
The invention does not need to add a diluting solvent, and the preparation process is more environment-friendly and pollution-free.
The whole preparation process does not need to add a metal catalyst (free radical photoinitiator), and the carbonized final product has high purity.
In the ultraviolet light photoinitiation vinyl crosslinking process in the step (1), the power of an ultraviolet gun is 50-300W, the distance is 5-10cm, and the initiation time is 1-30 min.
The invention can rapidly crosslink vinyl groups to form a vinyl crosslinking network within five minutes, improves the efficiency, does not need high-temperature curing, is not easy to generate gummosis phenomenon, reduces the energy consumption, and is one of the innovation points of the invention.
In addition, the vinyl crosslinking assistant with a special structure, furfural and phenol are used for initiating a crosslinking reaction in a chain manner, so that the reaction efficiency is greatly improved.
The thermal initiation of the phenol furfural condensation reaction by the photoinitiation reaction is another invention point of the invention.
The material is fixed using a mold in the phenolic condensation reaction.
In the step (2), the light carbon fiber/carbon composite thermal field curing material is fixed by using a self-made carbon/carbon mold and carbon fiber rope fixing combination mode, so that deformation in the high-temperature carbonization and graphitization processes is prevented. The hollow carbon/carbon mould can make full use of leftover materials left in the processing process, reduce the cost and ensure the quality of products. The invention also provides a novel point of the invention by using the wheel-shaped hollow supporting die.
In the step (2), the temperature in the carbonization process is 400-600 ℃. Vacuumizing in the carbonization process.
In the step (2), the temperature of the graphitization process is 2000-2800 ℃. The heating rate is 50-200 ℃/h.
In the step (3), the graphite adhesive system is sprayed in a spraying mode, and a high-temperature curing step is not needed, so that the processing efficiency is improved.
In the step (4), the light carbon fiber/carbon cylinder thermal field material with the graphite coating coated on the surface is purified in a mode of combining high temperature and chemical gas (fluoride), and the purification effect is good.
The proportion of the purified chemical gas to the light carbon fiber/carbon cylinder thermal field material coated with the graphite coating on the surface is (0.1-3): 100. the combination of high temperature and chemical gas (fluoride) for purification is also an innovation of the invention.
The light carbon fiber/carbon cylinder thermal field material with the graphite coating coated on the surface (see the detailed light carbon fiber/carbon cylinder thermal field material with the graphite coating coated on the surface in the attached figure 3) has the following advantages:
(1) low density and high strength
According to the invention, through the double-network crosslinking effect of the furfural phenol resin, the phenol furfural resin has high crosslinking density, the resin is tightly combined with the carbon fiber, the intermolecular distance is small, and the finally carbonized and graphitized material has low density, high mechanical property and high material strength, and is beneficial to operation and use. The density of the material can be controlled between 0.14 and 0.20g/cm3The bending strength can reach 3.5 MPa.
(2) High purity
According to the invention, by selecting a novel resin system, combining a polymer precursor method and a photo-initiated crosslinking method, no metal catalyst is required to be added in the curing process of phenol furfural, the obtained material has high purity after carbonization and graphitization, and simultaneously the impurity content in the graphite coating is low, and the final impurity content can be controlled below 10 ppm.
(3) Environment-friendly
A small molecular compound system is used in the preparation process, so that the preparation method is easy to impregnate, the problem that conventional resin is high in viscosity and difficult to impregnate is solved, meanwhile, no solvent is polluted in the reaction process, and the graphite coating is also an environment-friendly water-based resin system and is very environment-friendly.
(4) High efficiency and low energy consumption
In the preparation process, a resin system is impregnated by a spraying mode, the condensation reaction of phenol and furfural is initiated by the heat of photoinitiated crosslinking ethylene, heating and curing are not needed, the energy consumption is low, in addition, the photoinitiated crosslinking initiation rate is high, and vinyl crosslinking can be initiated within 5 minutes. Meanwhile, in the preparation process of the graphitized coating, a graphite adhesive system is sprayed in a spraying mode, and a high-temperature curing step is not needed, so that the processing efficiency is improved, and the energy consumption is reduced.
(5) Good heat insulation performance
The carbon fiber felt used in the invention has an X-Y-Z three-dimensional structure, so that the carbon fiber felt has high heat preservation performance, and the surface graphite coating can obstruct heat radiation in a high-temperature working environment through the action of reflection shielding, so that the heat insulation effect is further improved, and the carbon fiber felt has a low heat conductivity coefficient of 0.15W/(mK) (1000 ℃).
The light carbon fiber/carbon cylinder thermal field material with the graphite coating coated on the surface can be directly used in a high-temperature furnace protected by vacuum and inert gas, can be stably used at the temperature of 1000-2500 ℃, and is especially an indispensable thermal field cylinder material in high-temperature thermal fields such as a monocrystalline silicon straight-pull furnace thermal field, a silicon semiconductor crystal growth furnace thermal field, a silicon carbide semiconductor crystal growth furnace thermal field, an optical fiber drawing furnace thermal field, a sapphire crystal growth furnace thermal field and the like.
Drawings
FIG. 1 is an exemplary reaction process for a resin system according to the present invention;
FIG. 2 is a schematic diagram illustrating a process for preparing a lightweight carbon fiber/carbon cylindrical thermal field material with a graphite coating applied on the surface thereof according to the present invention;
fig. 3 is an example of the light carbon fiber/carbon cylinder thermal field material coated with graphite coating.
Detailed Description
The present invention will be described in further detail below by way of examples. However, the present invention is not limited to the following examples.
Example 1
The preparation method of the light carbon fiber/carbon cylinder thermal field material with the graphite coating coated on the surface comprises the following steps:
(1) spraying glue, dipping, curing and forming: (a) resin impregnation: winding a carbon fiber soft felt (100 parts) on a cylindrical metal mold, and then directly spraying and impregnating a resin system of phenol (10 parts), styrene (1 part), furfural (8 parts), ammonia water (0.4 part) and benzoin (0.1 part) with a spray gun; (b) ultraviolet light initiated double bond reaction: exciting a photoinitiator by ultraviolet light (100W, 5min), so that the initiator is in a free radical state or an excited state, then initiating a vinyl crosslinking reaction between the furfural resin and the vinyl co-crosslinking agent to form a vinyl crosslinking network, and simultaneously discharging a large amount of reaction heat; (c) phenol furfural condensation reaction: the vinyl crosslinking reaction heat promotes ammonia water to initiate phenol furfural polycondensation crosslinking reaction of furfural and phenol compounds to form a phenolic crosslinking network, and the vinyl crosslinking network and the phenolic crosslinking network are crossed with each other to form a double-crosslinking cured product.
(2) Carbonization and graphitization: removing the metal mould from the carbon fiber felt solidified product, installing a carbon/carbon mould, supporting the mould into 3 blocks, and ensuring that the area of a supporting barrel is about 1/3 of the total area; and binding carbon fiber ropes on the outer surface, wherein the distance between the carbon fiber ropes is 5cm, directly carrying out carbonization and graphitization reaction in a high-temperature furnace, and quickly preparing the light carbon fiber/carbon cylinder composite thermal field blank material. The heating rate is 100 ℃/h, the carbonization temperature is 600 ℃, and the carbonization time is 2 h; the graphitization temperature is 2000 ℃, and the graphitization time is 2 h.
(3) Graphitizing the coating: processing the light carbon fiber/carbon cylinder composite thermal field blank material to the required size, and then spraying a surface graphite coating system material by using a spray gun, wherein the parts of graphite flakes are 100 parts, the parts of polyvinyl butyral are 10 parts, and the parts of a phenolic resin aqueous solution are 200 parts. The thickness of the coating material was 200 um.
(4) And (3) purification: and (3) putting the carbon fiber/carbon cylinder thermal field material coated with the graphitized coating into a purification furnace for purification treatment, and discharging to obtain the light carbon fiber/carbon cylinder thermal field material coated with the graphite coating on the surface. Wherein the purified gas is fluoride, and the mass ratio of the fluoride to the light carbon fiber/carbon cylinder thermal field material with the graphite coating coated on the surface is 1: 100, the treatment temperature is 2400 ℃, and the treatment time is 2 h.
The bending strength of the light carbon fiber/carbon cylinder thermal field material with the final surface coated with the graphite coating is 3.5MPa, and the density can be controlled to be 0.15g/cm3The impurity content is 5ppm, and the thermal conductivity is 0.15W/(mK).
Example 2
The preparation method of the light carbon fiber/carbon cylinder thermal field material with the graphite coating coated on the surface comprises the following steps:
(1) spraying glue, dipping, curing and forming: (a) resin impregnation: winding a carbon fiber soft felt (100 parts) on a cylindrical metal mold, and then directly spraying and impregnating a resin system of phenol (20 parts), tripropylene glycol diallyl ether ester (2 parts), furfural (16 parts), ammonia water (0.8 part) and diphenylethanone (0.2 part) with a spray gun; (b) ultraviolet light initiated double bond reaction: exciting a photoinitiator by ultraviolet light (100W, 10min), so that the initiator is in a free radical state or an excited state, then initiating a vinyl crosslinking reaction between the furfural resin and the vinyl co-crosslinking agent to form a vinyl crosslinking network, and simultaneously discharging a large amount of reaction heat; (c) phenol furfural condensation reaction: the vinyl crosslinking reaction heat promotes ammonia water to initiate phenol furfural polycondensation crosslinking reaction of furfural and phenol compounds to form a phenolic crosslinking network, and the vinyl crosslinking network and the phenolic crosslinking network are crossed with each other to form a double-crosslinking cured product.
(2) Carbonization and graphitization: removing the metal mould from the carbon fiber felt solidified product, installing a carbon/carbon mould, supporting the mould into 3 blocks, and ensuring that the area of a supporting barrel is about 1/3 of the total area; and binding carbon fiber ropes on the outer surface, wherein the distance between the carbon fiber ropes is 5cm, directly carrying out carbonization and graphitization reaction in a high-temperature furnace, and quickly preparing the light carbon fiber/carbon cylinder composite thermal field blank material. The heating rate is 100 ℃/h, the carbonization temperature is 600 ℃, and the carbonization time is 2 h; the graphitization temperature is 2000 ℃, and the graphitization time is 2 h.
(3) Graphitizing the coating: processing the light carbon fiber/carbon cylinder composite thermal field blank material to the required size, and then spraying a surface graphite coating system material by using a spray gun, wherein the parts of graphite flakes are 100 parts, the parts of polyvinyl butyral are 15 parts, and the parts of a phenolic resin aqueous solution are 300 parts. The thickness of the coating material was 200 um.
(4) And (3) purification: and (3) putting the carbon fiber/carbon cylinder thermal field material coated with the graphitized coating into a purification furnace for purification treatment, and discharging to obtain the light carbon fiber/carbon cylinder thermal field material coated with the graphite coating on the surface. Wherein the purified gas is fluoride, and the mass ratio of the fluoride to the light carbon fiber/carbon cylinder thermal field material with the graphite coating coated on the surface is 0.8: 100, the treatment temperature is 2400 ℃, and the treatment time is 2 h.
The bending strength of the light carbon fiber/carbon cylinder thermal field material with the final surface coated with the graphite coating is 4.1MPa, and the density can be controlled to be 0.17g/cm3The impurity content is 7ppm, and the thermal conductivity is 0.17W/(mK).
Example 3
The preparation method of the light carbon fiber/carbon cylinder thermal field material with the graphite coating coated on the surface comprises the following steps:
(1) spraying glue, dipping, curing and forming: (a) resin impregnation: winding a carbon fiber soft felt (100 parts) on a cylindrical metal mold, and then directly spraying and impregnating the carbon fiber soft felt with a resin system of phenol (30 parts), trimethylolpropane trimethacrylate tripropylene glycol diallyl ether ester (3 parts), furfural (24 parts), ammonia water (1.2 parts) and alpha-amine alkyl phenyl ketone (0.3 part) by using a spray gun; (b) ultraviolet light initiated double bond reaction: exciting a photoinitiator by ultraviolet light (100W, 10min), so that the initiator is in a free radical state or an excited state, then initiating a vinyl crosslinking reaction between the furfural resin and the vinyl co-crosslinking agent to form a vinyl crosslinking network, and simultaneously discharging a large amount of reaction heat; (c) phenol furfural condensation reaction: the vinyl crosslinking reaction heat promotes ammonia water to initiate phenol furfural polycondensation crosslinking reaction of furfural and phenol compounds to form a phenolic crosslinking network, and the vinyl crosslinking network and the phenolic crosslinking network are crossed with each other to form a double-crosslinking cured product.
(2) Carbonization and graphitization: removing the metal mould from the carbon fiber felt solidified product, installing a carbon/carbon mould, supporting the mould into 3 blocks, and ensuring that the area of a supporting barrel is about 1/3 of the total area; and binding carbon fiber ropes on the outer surface, wherein the distance between the carbon fiber ropes is 5cm, directly carrying out carbonization and graphitization reaction in a high-temperature furnace, and quickly preparing the light carbon fiber/carbon cylinder composite thermal field blank material. The heating rate is 100 ℃/h, the carbonization temperature is 600 ℃, and the carbonization time is 2 h; the graphitization temperature is 2000 ℃, and the graphitization time is 2 h.
(3) Graphitizing the coating: processing the light carbon fiber/carbon cylinder composite thermal field blank material to the required size, and then spraying a surface graphite coating system material by using a spray gun, wherein the parts of graphite flakes are 100 parts, the parts of polyvinyl butyral are 30 parts, and the parts of a phenolic resin aqueous solution are 400 parts. The thickness of the coating material was 200 um.
(4) And (3) purification: and (3) putting the carbon fiber/carbon cylinder thermal field material coated with the graphitized coating into a purification furnace for purification treatment, and discharging to obtain the light carbon fiber/carbon cylinder thermal field material coated with the graphite coating on the surface. Wherein the purified gas is fluoride, and the mass ratio of the fluoride to the light carbon fiber/carbon cylinder thermal field material with the graphite coating coated on the surface is 0.7: 100, the treatment temperature is 2400 ℃, and the treatment time is 2 h.
The bending strength of the light carbon fiber/carbon cylinder thermal field material with the final surface coated with the graphite coating is 4.5MPa, and the density can be controlled to be 0.19g/cm3The impurity content is 9ppm, and the thermal conductivity is 0.19W/(mK).
Comparative example 1
The preparation method of the light carbon fiber/carbon cylinder thermal field material with the graphite coating coated on the surface comprises the following steps:
(1) spraying glue, dipping, curing and forming: (a) resin impregnation: winding a carbon fiber soft felt (100 parts) on a cylindrical metal die, and then directly spraying and impregnating a resin system of phenol (10 parts), furfural (8 parts) and sodium hydroxide (0.4 part) with a spray gun; (b) heating to initiate phenol furfural condensation reaction: and (3) promoting sodium hydroxide to initiate the phenol furfural polycondensation crosslinking reaction of furfural and a phenol compound by heating to form a crosslinking cured product.
(2) Carbonization and graphitization: removing the metal mold from the carbon fiber felt cured product, and installing a cylindrical carbon/carbon mold; and (3) directly carrying out carbonization and graphitization reaction in a high-temperature furnace to quickly prepare the light carbon fiber/carbon cylinder composite thermal field blank material. The heating rate is 100 ℃/h, the carbonization temperature is 600 ℃, and the carbonization time is 2 h; the graphitization temperature is 2000 ℃, and the graphitization time is 2 h.
(3) Graphitizing the coating: processing the light carbon fiber/carbon cylinder composite thermal field blank material to the required size, and then brushing a graphite coating system material on the surface in a glue brushing mode, wherein the parts of graphite flakes are 100 parts, and the parts of phenolic resin aqueous solution are 200 parts. The thickness of the coating material was 200 um.
(4) And (3) purification: and (3) putting the carbon fiber/carbon cylinder thermal field material coated with the graphitized coating into a purification furnace for high-temperature purification treatment, and discharging to obtain the light carbon fiber/carbon cylinder thermal field material coated with the graphite coating on the surface. The treatment temperature was 2800 ℃ and the treatment time was 2 h.
The bending strength of the light carbon fiber/carbon cylinder thermal field material with the final surface coated with the graphite coating is 3.7MPa, and the density can be controlled to be 0.155g/cm3The impurity content is 600ppm, and the thermal conductivity is 0.16W/(mK). The impurity content of the finally prepared product is seriously exceeded, and the coating is easy to fall off. The energy consumption is increased by using a thermal curing mode for curing in the process; the use of cylindrical carbon/carbon molds during carbonization and graphitization increases mold cost; carbon fiber ropes are not used for binding in the carbonization and graphitization processes, so that the material is easy to expand and deform; the graphitized coating does not use a spraying method, so that the efficiency is low, and meanwhile, polyvinyl butyral is not added, so that the graphitized coating is easy to fall off; the purification process uses a high-temperature purification method, which consumes energy and has low purification efficiency.
Comparative example 2
The preparation method of the light carbon fiber/carbon cylinder thermal field material with the graphite coating coated on the surface comprises the following steps:
(1) spraying glue, dipping, curing and forming: (a) resin impregnation: winding a carbon fiber soft felt (100 parts) on a cylindrical metal die, and then directly spraying and impregnating a resin system of phenol (10 parts), styrene (1 part), furfural (8 parts) and sodium hydroxide (0.4 part) with a spray gun; (b) ultraviolet light initiated double bond reaction: without initiator, no reaction.
Until the reaction process, the liquid resin system cannot be crosslinked under the ultraviolet light initiation condition, the resin cannot be cured, the solid material cannot be prepared, and the sample preparation fails.

Claims (10)

1. The light carbon fiber/carbon cylinder thermal field material with the graphite coating coated on the surface is characterized in that the raw material composition and the mass portion for preparing the light carbon fiber/carbon cylinder thermal field material blank material comprise:
carbon fiber soft felt: 100 portions of
Phenol: 10-30 parts of
And (3) furfural: 8 to 24 portions of
Ammonia water: 0.4 to 1.2 portions of
Vinyl co-crosslinking agent: 1-3 parts of
Photoinitiator (2): 0.1-0.3 part;
the preparation method of the light carbon fiber/carbon cylinder thermal field material with the graphite coating coated on the surface comprises the following steps:
(1) spraying glue, dipping, curing and forming: (a) resin impregnation: winding the carbon fiber soft felt on a cylindrical metal die, and then directly spraying and impregnating the carbon fiber soft felt by using a resin system of phenol, a vinyl auxiliary crosslinking agent, furfural, ammonia water and a photoinitiator; (b) ultraviolet light initiated double bond reaction: initiating a vinyl crosslinking reaction between the furfural resin and a vinyl auxiliary crosslinking agent by exciting a photoinitiator through ultraviolet light to form a vinyl crosslinking network; (c) phenol furfural condensation reaction: the vinyl crosslinking reaction heat promotes ammonia water to initiate phenol furfural polycondensation crosslinking reaction of furfural and phenol compounds to form a phenolic crosslinking network, and the vinyl crosslinking network and the phenolic crosslinking network are crossed with each other to form a double-crosslinking cured product;
(2) carbonization and graphitization: removing the metal mold from the carbon fiber felt cured product, mounting a carbon/carbon mold, binding a carbon fiber rope on the outer surface, and directly performing carbonization and graphitization reaction to prepare a light carbon fiber/carbon cylinder composite thermal field blank material;
(3) graphitizing the coating: processing the light carbon fiber/carbon cylinder composite thermal field blank material to a required size, and then spraying a graphite coating system material on the surface;
(4) and (3) purification: and purifying the carbon fiber/carbon cylinder thermal field material coated with the graphitized coating to obtain the light carbon fiber/carbon cylinder thermal field material coated with the graphite coating on the surface.
2. The light carbon fiber/carbon cylinder thermal field material with the graphite coating coated on the surface as claimed in claim 1, wherein the carbon fiber soft felt is a carbon fiber soft felt treated by a silane coupling agent, the carbon fiber soft felt is prepared by subjecting long carbon fibers to an air-laying and needle-punching felt forming process, and the ratio of Z-direction fibers to X-Y in-plane fibers of the activated carbon fiber soft felt is 1: (50-150) the density is 500-700 g/cm2The thickness is 10 +/-1 mm; the length of the long carbon fiber is 10-15 cm.
3. The light carbon fiber/carbon cylinder thermal field material with the graphite coating coated on the surface thereof as claimed in claim 1, wherein the vinyl auxiliary crosslinking agent is a vinyl bond-containing mono-ethylene low molecular compound, a divinyl crosslinking agent or a polyvinyl crosslinking agent; wherein the monoethylene low molecular compound is styrene or acrylate; the divinyl crosslinking agent is tripropylene glycol dipropylene ether ester; the polyvinyl crosslinking agent is trimethylolpropane triacrylate, trimethylolpropane trimethacrylate or triallyl isocyanurate.
4. The light-weight carbon fiber/carbon cylinder thermal field material with the graphite coating coated on the surface thereof as claimed in claim 1, wherein the photoinitiator is a free radical photoinitiator or a cationic photoinitiator; wherein the free radical photoinitiator is benzoin butyl ether, benzoin dimethyl ether, benzoin ethyl ether, benzoin isopropyl ether, alpha-dimethoxy-alpha-phenylacetophenone, diphenylethanone, alpha-hydroxyalkylphenone, alpha-aminoalkylphenone, alpha-diethoxyacetophenone, bisbenzoylphenylphosphine oxide, aroylphosphine oxide, 2, 4-dihydroxybenzophenone, benzophenone, thiopropoxythioxanthone or isopropylthioxanthone;
the cationic photoinitiator is diaryl iodonium salt, triaryl iodonium salt, alkyl iodonium salt or cumeneferrocenyl hexafluorophosphate.
5. The light carbon fiber/carbon cylinder thermal field material with the graphite coating coated on the surface as claimed in any one of claims 1 to 4, characterized in that the raw material composition for preparing the surface graphite coating material and the parts by mass thereof comprise:
graphite flake: 100 portions of
Polyvinyl butyral: 10-30 parts of
Phenolic resin aqueous solution: 200 portions and 600 portions.
6. The light-weight carbon fiber/carbon cylindrical thermal field material with a graphite coating coated on the surface thereof as claimed in claim 5, wherein the graphite sheet has a size of 30-80um and a thickness of 10 um; the polyvinyl butyral is chemically pure; the phenolic resin aqueous solution is a mixture of water-soluble phenolic resin and water, wherein the solid content is 40-75%.
7. The method for preparing the light carbon fiber/carbon cylinder thermal field material with the graphite coating coated on the surface, which is characterized by comprising the following steps:
(1) spraying glue, dipping, curing and forming: (a) resin impregnation: winding the carbon fiber soft felt on a cylindrical metal die, and then directly spraying and impregnating the carbon fiber soft felt by using a resin system of phenol, a vinyl auxiliary crosslinking agent, furfural, ammonia water and a photoinitiator; (b) ultraviolet light initiated double bond reaction: initiating a vinyl crosslinking reaction between the furfural resin and a vinyl auxiliary crosslinking agent by exciting a photoinitiator through ultraviolet light to form a vinyl crosslinking network; (c) phenol furfural condensation reaction: the vinyl crosslinking reaction heat promotes ammonia water to initiate phenol furfural polycondensation crosslinking reaction of furfural and phenol compounds to form a phenolic crosslinking network, and the vinyl crosslinking network and the phenolic crosslinking network are crossed with each other to form a double-crosslinking cured product;
(2) carbonization and graphitization: removing the metal mold from the carbon fiber felt cured product, mounting a carbon/carbon mold, binding a carbon fiber rope on the outer surface, and directly performing carbonization and graphitization reaction to prepare a light carbon fiber/carbon cylinder composite thermal field blank material;
(3) graphitizing the coating: processing the light carbon fiber/carbon cylinder composite thermal field blank material to a required size, and then spraying a graphite coating system material on the surface;
(4) and (3) purification: and purifying the carbon fiber/carbon cylinder thermal field material coated with the graphitized coating to obtain the light carbon fiber/carbon cylinder thermal field material coated with the graphite coating on the surface.
8. The method for preparing the light carbon fiber/carbon cylinder thermal field material with the graphite coating coated on the surface, as claimed in claim 7, is characterized in that in the step (1), the mass concentration of the ammonia water is 10-100%, the power of an ultraviolet gun is 50-300W, the distance is 5-10cm, and the initiation time is 1min-30min in the process of initiating vinyl crosslinking through ultraviolet light.
9. The method for preparing the light carbon fiber/carbon cylinder thermal field material with the graphite coating coated on the surface according to the claim 7, characterized in that in the step (2), the temperature in the carbonization process is 400-600 ℃, and the vacuum pumping is performed in the carbonization process;
the temperature of the graphitization process is 2000-2800 ℃; the heating rate is 50-200 ℃/h;
the carbon/carbon mold is a wheel-shaped hollow support mold.
10. The method for preparing the light carbon fiber/carbon cylinder thermal field material with the graphite coating coated on the surface thereof as claimed in claim 7, wherein in the step (4), the light carbon fiber/carbon cylinder thermal field material with the graphite coating coated on the surface is purified by using a combination of temperature rise and addition of gas fluoride;
the mass ratio of the fluoride to the light carbon fiber/carbon cylinder thermal field material with the graphite coating coated on the surface is (0.1-3): 100.
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