CN112591729B - Cured carbon fiber felt and preparation method thereof - Google Patents
Cured carbon fiber felt and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a cured carbon fiber felt and a preparation method thereof. The method is mainly based on the foaming principle to realize the uniform distribution of the carbon fibers in the cured carbon fiber felt and obtain the cured carbon fiber felt with very low density, and the density of the cured carbon fiber felt is 0.18g/cm 3 ～0.22g/cm 3 The heat conductivity coefficient is 0.19W/mk to 0.22, the ash content is less than or equal to 28ppm, and the specific heat is 0.35 to 0.65J/g.k; is particularly suitable for vacuum resistance furnacesAnd in thermal fields such as induction furnaces, sintering furnaces, heat treatment furnaces and the like.
Description
Technical Field
The invention relates to a carbon felt, in particular to a low-density and high-heat-property cured carbon fiber felt and a preparation method thereof, belonging to the technical field of carbon felt preparation.
Background
In halfThe conductor and solar industries, single crystal silicon and polycrystalline silicon are important semiconductor materials. In industrial production, single crystal silicon and polycrystalline silicon for semiconductors and solar energy are required to have very high purity. Therefore, in the high-temperature furnace for producing monocrystalline silicon and polycrystalline silicon, the thermal insulation material of the high-temperature furnace generally adopts carbon fiber felt as a thermal insulation layer. The carbon fiber felt is divided into a soft felt and a cured carbon felt, wherein the soft felt is a felt formed by directly needling carbon fibers and has the density of 0.1g/cm 3 The texture is softer below. The cured carbon felt is prepared by coating the surface of carbon fiber with pyrolytic resin carbon on the basis of soft felt, and has a density of 0.3g/cm 3 Above, the texture is harder. Compared with soft felt, the cured carbon felt has the advantages of low volatility, self-supporting function, convenience in installation and replacement and the like, and is widely applied to vacuum high-temperature furnaces and inert atmosphere protection furnaces.
Currently, there are three methods for preparing cured carbon mats. Firstly, a plurality of layers of soft felts are laminated and then dipped into a resin solution, and then are drained and carbonized. Secondly, resin is coated on the surface of the soft felt in a brush way, and then the resin is bonded layer by layer and carbonized to obtain the cured carbon felt. Thirdly, the carbon fiber net tire is needled into a corresponding mould layer by layer, is taken out for short-time carbon vapor deposition, and is machined to obtain the solidified carbon fiber felt. In the first method, the fiber density of the contact area of the multi-layer soft felt lamination is high, resin is easy to accumulate, and the cured carbon felt has uneven density and poor heat insulation performance. In the second method, because the resin is coated on the surface of the soft felt, the resin content in the soft felt is little or no resin exists, so that the self-supporting property of the prepared cured carbon felt is weak, and the mounting precision is influenced. The third method is difficult to manufacture large and special-shaped products, and has high production cost, long cycle and difficult density control.
Chinese patent CN100567217C provides a preparation method of a high-purity solidified carbon felt for a silicon crystal growing furnace, and the high-temperature pretreatment makes the product become a graphite felt body; manufacturing a blank body by using a graphite felt body; curing and shaping the blank body uniformly permeated with the curing agent; carbonizing the blank; then carrying out chemical vapor predeposition on the blank; performing mechanical cutting on the surface of part to be cut; and then the blank is processed at high temperature. The solidified carbon felt prepared by the method has the advantages of low heat conductivity coefficient, good energy-saving and heat-preserving effects, light weight, high strength, stable quality, reliable use and controllable metal impurity content within 300ppm or even 100ppm, but still has the defects of complex product preparation process and poor product heat-preserving effect.
Chinese patent CN202430447U proposes an equipment of thick felt of two-sided oblique thorn preparation pre-oxidation silk, and the elevating system drive is connected the lifter plate the utility model discloses a two-sided acupuncture equipment saves process flow, and the homogeneity is strong, and convenient operation can continuous production, and production efficiency is high, is fit for batch production. However, the preparation process of the equipment is still the traditional carbon felt production process, and the defects of complex process and poor product heat preservation effect exist in the production process.
Chinese patent CN102505340A proposes a method for preparing a pre-oxidized fiber thick felt, the pre-oxidized fiber thick felt with good uniformity can be prepared by the method, and a carbon fiber heat insulation felt with excellent heat insulation performance and long service life can be obtained after carbonization treatment and high-temperature treatment in the later period. The equipment disclosed by the invention is simple in structure, simple to operate, capable of realizing continuous production, high in production efficiency and suitable for batch production. However, the method still has the defects of poor product performance, limited production continuity and the like.
Disclosure of Invention
In view of the drawbacks of the prior art cured carbon fiber mats, it is a first object of the present invention to provide a cured carbon fiber mat having a low density and high thermal properties, the cured carbon fiber mat having a density of 0.18g/cm 3 ～0.22g/cm 3 The heat conductivity coefficient is 0.19W/mk-0.22W/mk, the ash content is less than or equal to 28ppm, and the specific heat is 0.35J/g.k-0.65J/g.k, so that the application requirements in thermal fields such as vacuum resistance furnaces, induction furnaces, sintering furnaces, heat treatment furnaces and the like are met.
The second purpose of the invention is to provide a method for preparing the solidified carbon fiber felt based on the foaming principle, which has simple steps and low cost and is suitable for industrial production.
In order to achieve the technical purpose, the invention provides a preparation method of a cured carbon fiber felt, which comprises the following steps:
1) Stirring and mixing a mixture A consisting of polyether propylene glycol, polyether glycerol and carbon fibers, a mixture B consisting of liquid resin, an organic solvent and carbon fibers and a mixture C consisting of polymethylene polyphenyl polyisocyanate, the organic solvent and the carbon fibers, and carrying out prepolymerization reaction to obtain a prepolymer;
2) Transferring the prepolymer into a mold for foaming and curing to obtain a cured carbon fiber felt precursor;
3) And carbonizing and graphitizing the cured carbon fiber precursor to obtain the cured carbon fiber felt.
The technical scheme of the invention prepares the cured carbon fiber felt material by a foaming method, and has the greatest advantage that the density of the precursor can be greatly reduced so as to obtain the cured carbon fiber felt with low density, and the density reaches 0.18g/cm 3 ～0.22g/cm 3 The density of the cured carbon fiber prepared by the conventional method is far lower than that of the cured carbon fiber prepared by the conventional method by 0.3g/cm 3 Meanwhile, the carbon fibers can be uniformly dispersed in the precursor material through a foaming method, so that the carbon fiber phase is uniformly distributed in the cured carbon fiber felt, the functions and the effects of the carbon fiber phase can be better exerted, and the cured carbon fiber felt material with better thermal properties can be obtained.
As a preferable scheme, the mixture A consists of polyether propylene glycol, polyether glycerol and carbon fiber in a mass ratio of 1-2.
As a preferable scheme, the moisture mass fraction of the A mixed material is less than or equal to 5%, and the pH value is 5.5-7.5.
As a preferable scheme, the B mixture is composed of liquid resin, an organic solvent, a foaming agent and carbon fiber according to a mass ratio of 4.
As a preferred embodiment, the liquid resin is at least one of phenolic resin, furan resin, epoxy resin, polyamide resin, urea resin and polyurethane resin.
As a preferable embodiment, the organic solvent is at least one of absolute alcohol, acetone, isopropyl alcohol, diethyl ether and propylene oxide.
As a preferable scheme, the C mixed material consists of polymethylene polyphenyl polyisocyanate, an organic solvent and carbon fiber according to the mass ratio of 2-5.
As a preferable embodiment, the organic solvent is at least one of absolute alcohol, acetone, isopropyl alcohol, diethyl ether and propylene oxide.
As a preferable scheme, the mixing mass ratio of the mixture A, the mixture B and the mixture C is 1:1 to 1.4:1.05 to 1.85.
Preferably, the carbon fiber chopped carbon fiber has a length of 10 to 500mm. The optimized chopped carbon fibers can be dispersed into a larger volume space along with the foaming material, so that the carbon fibers can be more uniformly distributed in the cured carbon fiber felt precursor, and the low density and high heat performance of the cured carbon fiber felt after later carbonization and graphitization are realized.
In the preparation process of the solidified carbon fiber felt, the mixture A is a foaming main body, the mixture B is a main carbon source, the mixture C is a catalyst, and after the mixture A, the mixture B and the mixture C are mixed, the mixture A generates chain growth, foaming, crosslinking, solidification and other reactions under the action of the mixture C, so that the mixture A can expand and foam rapidly; the mixture B is used as an additive, is a main carbon source in the later carbonization process, and provides mechanical support for the carbonized low-density cured carbon fiber felt product.
As a preferable scheme, the temperature of the prepolymerization reaction is 15-95 ℃ and the time is 10-60 minutes.
As a preferable scheme, the foaming and curing time is 20 minutes to 120 minutes;
preferably, the carbonization temperature is 500-1100 ℃ and the time is 1-3 hours.
In a preferred embodiment, the graphitization temperature is 1800-2400 ℃ and the time is 1-3 hours.
In the technical scheme of the invention, the heating rate in the carbonization and graphitization treatment process is as follows: 1-8 ℃/min.
The mould provided by the invention is a common mould meeting high temperature resistance requirements in the industry, such as a graphite material mould, a steel product and the like, and an inner cavity of the mould is designed according to the shape of a cured carbon fiber felt. The inner surface of the mould is lined with a demoulding material, which is commonly carbon cloth, graphite paper, carbon fiber net tyre and the like, and can be used alone or in combination.
The density of the cured carbon fiber felt precursor prepared by the foaming method is 0.22g/cm 3 ～0.30g/cm 3 The density of the obtained solidified carbon fiber felt is 0.18g/cm through further high-temperature carbonization and graphitization treatment 3 ～0.22g/cm 3 。
The invention also provides a cured carbon fiber felt which is obtained by the preparation method.
As a preferable mode, the density of the cured carbon fiber felt is 0.18g/cm 3 ～0.22g/cm 3 The heat conductivity coefficient is 0.19W/mk to 0.22W/mk, the ash content is less than or equal to 28ppm, and the specific heat is 0.35J/g.k to 0.65J/g.k.
The invention provides a preparation method of a cured carbon fiber felt, which comprises the following steps:
(1) Selecting a mould made of a proper material (such as a graphite material, a steel material and the like), and lining a demoulding material on the inner surface of the mould, wherein the demoulding material is specifically selected from carbon cloth, graphite paper, a carbon fiber net tire and the like;
(2) Mixing polyether propylene glycol, polyether glycerol and carbon fiber according to a mass ratio of 1-2; wherein the carbon fiber is chopped carbon fiber with the length of 10-500 mm; the mixture A meets the conditions that the water mass fraction is less than or equal to 5 percent and the pH value is 5.5-7.5;
(3) Mixing and stirring liquid resin, an organic solvent and carbon fiber according to a mass ratio of 4; the liquid resin can be selected from phenolic resin, furan resin, epoxy resin, polyamide resin, urea resin or polyurethane resin; the organic solvent is absolute alcohol, acetone, isopropanol, diethyl ether or propylene oxide, etc.; the carbon fiber is chopped carbon fiber with the length of 10-500 mm;
(4) Mixing and stirring polymethylene polyphenyl polyisocyanate, an organic solvent and carbon fiber according to a mass ratio of 2-5; wherein the organic solvent is absolute alcohol, acetone, isopropanol, diethyl ether or propylene oxide; the carbon fiber is chopped carbon fiber with the length of 10-500 mm;
(5) The mixture A, the mixture B and the mixture C are mixed according to the mass ratio of 1:1 to 1.4:1.05 to 1.85, adding the mixture into a mixer with an electric stirrer, stirring the mixture for 10 to 60 minutes at the temperature of between 15 and 95 ℃, pouring the mixture into a mould for foaming and curing for 20 to 120 minutes, taking a foam out of the mould, wherein the density of the foam is 0.22g/cm 3 ～0.30g/cm 3 Preparing a precursor of the solidified carbon fiber felt with a corresponding shape;
(6) And (3) putting the cured carbon fiber precursor sample into a vacuum furnace, heating to the carbonization temperature at the speed of 1-8 ℃/min, carbonizing at 500-1100 ℃, preserving heat for 1-3 hours, continuously heating to a higher temperature, graphitizing at 1800-2400 ℃, and preserving heat for 1-2 hours to obtain the cured carbon fiber felt.
Compared with the prior art, the technical scheme of the invention has the following beneficial effects:
(1) The high-curing carbon fiber felt provided by the invention has a unique low-density structure, and carbon fibers are uniformly distributed in the felt body, so that the high-curing carbon fiber felt has excellent thermal properties, for example, the density of a cured carbon fiber felt material is 0.18g/cm 3 ～0.22g/cm 3 The heat conductivity coefficient is 0.19W/mk to 0.22W/mk, the ash content is less than or equal to 28ppm, the specific heat is 0.35J/g.k to 0.65J/g.k, the corresponding parameters are all superior to the carbon felt material for the industrial production at the present stage, the density is reduced by 5 to 8 times, the heat conductivity coefficient is improved by more than 10 times, and the ash content is reduced by 50 to 60 times; the specific heat quantity is reduced by more than 20 times, and the method has great commercial application value.
(2) The preparation method is simple to operate, low in cost and easy for industrial production;
(3) The cured carbon fiber felt meets the application requirements in thermal fields such as vacuum resistance furnaces, induction furnaces, sintering furnaces, heat treatment furnaces and the like.
Detailed Description
The following examples further illustrate the invention.
While the following is a description of the preferred embodiments of the present invention, it should be noted that those skilled in the art can make various modifications and adaptations without departing from the principle of the present invention, and such modifications and adaptations are intended to be within the scope of the present invention as set forth in the following claims.
In each example, the raw materials used were all common commercial products.
Example 1
A preparation method of a high-performance cured carbon fiber felt comprises the following steps:
(1) Selecting a mould for curing the carbon fiber felt which meets the requirement of a thermal field, and lining a demoulding material on the inner surface of the mould, wherein the demoulding material is carbon cloth.
(2) Adding polyether propylene glycol, polyether glycerol and carbon fiber, mixing and stirring according to the mass ratio of 1.2.
(3) Mixing and stirring liquid phenolic resin, absolute ethyl alcohol and carbon fiber according to a mass ratio of 4;
(4) Mixing and stirring polymethylene polyphenyl polyisocyanate, absolute ethyl alcohol and carbon fiber according to a mass ratio of 2.
(5) The mixture A, the mixture B and the mixture C are mixed according to the mass ratio of 1:1.4:1.05, adding the mixture into a mixer with an electric stirrer, stirring at 15 ℃ for 10 minutes, pouring the mixture into the mould in the step (1), foaming and curing, and taking out a foam from the mould after 20 minutes to prepare the cured carbon fiber felt precursor with the corresponding shape. The density of the cured carbon fiber felt is 0.3g/cm 3 。
(6) And (3) putting the cured carbon fiber precursor sample into a vacuum furnace, wherein the temperature rise rate is 1 ℃/min, the carbonization temperature of the vacuum furnace is 500 ℃, the carbonization heat preservation time is 1 hour, the temperature is continuously raised to 1800 ℃ for graphitization, and the graphitization heat preservation time is 1 hour, so that the cured carbon fiber felt is obtained.
As shown in Table 1, the amount of the cured carbon fiber felt carbon fiber produced was 0.18g/cm 3 The thermal conductivity was 0.21W/mk, the ash content was 15ppm, and the specific heat was 0.36J/g.k.
Example 2
A preparation method of a high-performance cured carbon fiber felt comprises the following steps:
(1) Selecting a mould for curing the carbon fiber felt meeting the thermal field requirement, and lining a demoulding material on the inner surface of the mould, wherein the demoulding material is carbon cloth.
(2) Adding polyether propylene glycol, polyether glycerol and carbon fiber, mixing and stirring according to the mass ratio of 1.5.
(3) Mixing and stirring liquid furan resin, acetone and carbon fiber according to a mass ratio of 4;
(4) Mixing and stirring polymethylene polyphenyl polyisocyanate, acetone and carbon fiber according to a mass ratio of 2.5.
(5) The mixture A, the mixture B and the mixture C are mixed according to the mass ratio of 1:1:1.5, adding the mixture into a mixer with an electric stirrer, stirring at 35 ℃ for 20 minutes, pouring the mixture into the mould in the step (1), foaming and curing the mixture, taking out the foam from the mould after 40 minutes to prepare a cured carbon fiber felt precursor with a corresponding shape, wherein the density of the cured carbon fiber felt is 0.25g/cm 3 。
(6) And (3) putting the cured carbon fiber precursor sample into a vacuum furnace, wherein the temperature rise rate is 3 ℃/min, the carbonization temperature of the vacuum furnace is 600 ℃, the carbonization heat preservation time is 1.5 hours, the temperature is continuously raised to 1850 ℃, graphitization is carried out, and the graphitization heat preservation time is 1.25 hours, thus obtaining the cured carbon fiber felt.
As shown in Table 1, the cured carbon fiber felt prepared in this example had a density of 0.18g/cm 3 The thermal conductivity coefficient is 0.22W/mk, the ash content is 18ppm, and the specific heat is 0.38J/g.k.
Example 3
A preparation method of a high-performance cured carbon fiber felt comprises the following steps:
(1) Selecting a mould of the solidified carbon fiber felt which meets the requirement of a thermal field, and lining a demoulding material on the inner surface of the mould, wherein the demoulding material is graphite paper.
(2) And adding polyether propylene glycol, polyether glycerol and carbon fiber, mixing and stirring according to a mass ratio of 1.8.
(3) Mixing and stirring liquid epoxy resin, isopropanol and carbon fiber according to a mass ratio of 4;
(4) Mixing and stirring polymethylene polyphenyl polyisocyanate, isopropanol and carbon fiber according to a mass ratio of 2.
(5) The mixture A, the mixture B and the mixture C are mixed according to the mass ratio of 1:1.2:1.6, adding the mixture into a mixer with an electric stirrer, stirring at 55 ℃ for 30 minutes, pouring the mixture into the mould in the step (1), foaming and curing the mixture, taking out the foam from the mould after 60 minutes to prepare a cured carbon fiber felt precursor with a corresponding shape, wherein the density of the cured carbon fiber felt is 0.22g/cm 3 。
(6) And (3) putting the cured carbon fiber precursor sample into a vacuum furnace, wherein the temperature rise rate is 5 ℃/min, the carbonization temperature of the vacuum furnace is 700 ℃, the carbonization heat preservation time is 2 hours, the temperature is continuously raised to 1800 ℃ for graphitization, and the graphitization heat preservation time is 1.5 hours, so that the cured carbon fiber felt is obtained.
As shown in Table 1, the cured carbon fiber felt prepared in this example had a density of 0.18g/cm 3 The thermal conductivity was 0.19W/mk, the ash content was 28ppm, and the specific heat was 0.35J/g.k.
Example 4
A preparation method of a high-performance cured carbon fiber felt comprises the following steps:
(1) Selecting a mould of the solidified carbon fiber felt which meets the requirement of a thermal field, and lining a demoulding material on the inner surface of the mould, wherein the demoulding material is graphite paper.
(2) Adding polyether propylene glycol, polyether glycerol and carbon fiber, mixing and stirring according to the mass ratio of 1.
(3) Mixing and stirring liquid polyamide resin, diethyl ether and carbon fiber according to a mass ratio of 4;
(4) Mixing and stirring polymethylene polyphenyl polyisocyanate, diethyl ether and carbon fiber according to a mass ratio of 2.
(5) The mixture A, the mixture B and the mixture C are mixed according to the mass ratio of 1:1.2:1.8, adding the mixture into a mixer with an electric stirrer, stirring at 75 ℃ for 40 minutes, pouring the mixture into the mould in the step (1), foaming and curing the mixture, taking out a foam from the mould after 80 minutes to prepare a cured carbon fiber felt precursor with a corresponding shape, wherein the density of the cured carbon fiber felt is 0.27g/cm 3 。
(6) And (3) putting the cured carbon fiber precursor sample into a vacuum furnace, wherein the temperature rise rate is 7 ℃/min, the carbonization temperature of the vacuum furnace is 900 ℃, the carbonization heat preservation time is 2.5 hours, the temperature is continuously raised to 2300 ℃ for graphitization, and the graphitization heat preservation time is 1.75 hours, so that the cured carbon fiber felt is obtained.
As shown in Table 1, the cured carbon fiber felt prepared in this example had a density of 0.19g/cm 3 The thermal conductivity was 0.21W/mk, the ash content was 23ppm, and the specific heat was 0.6J/g.k.
Example 5
A preparation method of a high-performance cured carbon fiber felt comprises the following steps:
(1) Selecting a mould for curing the carbon fiber felt meeting the requirement of a thermal field, and lining a demoulding material on the inner surface of the mould, wherein the demoulding material is a carbon fiber net tyre.
(2) And adding polyether propylene glycol, polyether glycerol and carbon fiber, mixing and stirring according to the mass ratio of 1.
(3) Mixing and stirring liquid polyurethane resin, epoxypropane and carbon fiber according to a mass ratio of 4;
(4) Mixing and stirring polymethylene polyphenyl polyisocyanate, propylene oxide and carbon fiber according to a mass ratio of 2.
(5) The mixture A, the mixture B and the mixture C are mixed according to the mass ratio of 1:1.4:1.85, adding into a mixer with an electric stirrer, stirring at 95 deg.C for 60 min, pouring the mixtureFoaming and curing in the mould in the step (1), taking out the foam from the mould after 120 minutes to prepare a cured carbon fiber felt precursor with a corresponding shape, wherein the density of the cured carbon fiber felt is 0.28g/cm 3 。
(6) And (3) putting the cured carbon fiber precursor sample into a vacuum furnace, wherein the temperature rise rate is 8 ℃/min in the whole process, the carbonization temperature of the vacuum furnace is 1100 ℃, the carbonization heat preservation time is 3 hours, the temperature is continuously raised to 2400 ℃ for graphitization, and the graphitization heat preservation time is 2 hours, so that the cured carbon fiber felt is obtained.
As shown in Table 1, the cured carbon fiber felt prepared in this example had a density of 0.20g/cm 3 The thermal conductivity was 0.20W/mk, the ash content was 25ppm, and the specific heat was 0.65J/g.k.
Comparative example 1
A preparation method of a cured carbon fiber felt comprises the following steps:
(1) Selecting a mould for curing the carbon fiber felt meeting the requirement of a thermal field, and lining a demoulding material on the inner surface of the mould, wherein the demoulding material is a carbon fiber net tyre.
(2) And adding epoxy resin, absolute ethyl alcohol and carbon fiber, mixing and stirring according to the mass ratio of 1.
(3) Adding the mixture obtained in the step (2) into a mixer with an electric stirrer, stirring at 95 ℃ for 120 minutes, pouring the obtained mixture into the mould obtained in the step (1), drying in a 60 ℃ oven, taking out the mixed solid from the mould after 600 minutes to obtain a solidified carbon fiber felt precursor with a corresponding shape, wherein the density of the solidified carbon fiber felt is 5g/cm 3 。
(4) And (3) putting the cured carbon fiber precursor sample into a vacuum furnace, wherein the temperature rise rate is 5 ℃/min in the whole process, the carbonization temperature of the vacuum furnace is 1100 ℃, the carbonization heat preservation time is 2 hours, the temperature is continuously raised to 2400 ℃ for graphitization, and the graphitization heat preservation time is 1 hour, so that the cured carbon fiber felt is obtained.
As shown in Table 1, the cured carbon fiber felt prepared in this example had a density of 2.1g/cm 3 The thermal conductivity was 1.3W/mk, the ash content was 344ppm, and the specific heat was 3.2J/g.k. This comparisonThe examples show that without the foaming process, the density in the cured carbon fiber mat is higher, the carbon fibers are not sufficiently dispersed, and the thermal properties are also poor.
Comparative example 2
A preparation method of the cured carbon fiber felt comprises the following steps:
(1) Selecting a mould for curing the carbon fiber felt which meets the requirement of a thermal field, and lining a demoulding material on the inner surface of the mould, wherein the demoulding material is a carbon fiber net tire.
(2) And adding epoxy resin, acetone and carbon fiber, mixing and stirring according to a mass ratio of 1.
(3) Adding the mixture obtained in the step (2) into a mixer with an electric stirrer, stirring at 85 ℃ for 100 minutes, pouring the obtained mixture into the mould in the step (1), drying in a 65 ℃ oven, taking out the solid mixture from the mould after 480 minutes to obtain a solidified carbon fiber felt precursor with a corresponding shape, wherein the density of the solidified carbon fiber felt is 4.8g/cm 3 。
(4) And (3) putting the cured carbon fiber precursor sample into a vacuum furnace, wherein the temperature rise rate is 4 ℃/min, the carbonization temperature of the vacuum furnace is 1000 ℃, the carbonization heat preservation time is 1 hour, continuously raising the temperature to 2300 ℃ for graphitization, and the graphitization heat preservation time is 2 hours, thus obtaining the cured carbon fiber felt.
As shown in Table 1, the cured carbon fiber felt prepared in this example had a density of 2.4g/cm 3 The thermal conductivity is 1.8W/mk, the ash content is 521ppm, and the specific heat is 3.1J/g.k.
This comparative example illustrates that without the foaming process, the density in the cured carbon fiber mat is higher, and the carbon fibers are not sufficiently dispersed, and the thermal properties are also poor.
Comparative example 3
A preparation method of a cured carbon fiber felt comprises the following steps:
(1) Selecting a mould for curing the carbon fiber felt which meets the requirement of a thermal field, and lining a demoulding material on the inner surface of the mould, wherein the demoulding material is a carbon fiber net tire.
(2) Adding phenolic resin, acetone and carbon fiber, mixing and stirring according to the mass ratio of 2.
(3) Adding the mixture obtained in the step (2) into a mixer with an electric stirrer, stirring at 105 ℃ for 60 minutes, pouring the obtained mixture into the mould obtained in the step (1), drying in an oven at 70 ℃, taking out the solid mixture from the mould after 600 minutes to obtain a solidified carbon fiber felt precursor with a corresponding shape, wherein the density of the solidified carbon fiber felt is 4.6g/cm 3 。
(4) And (3) putting the cured carbon fiber precursor sample into a vacuum furnace, wherein the temperature rise rate is 5 ℃/min in the whole process, the carbonization temperature of the vacuum furnace is 1100 ℃, the carbonization heat preservation time is 2 hours, the temperature is continuously raised to 2400 ℃ for graphitization, and the graphitization heat preservation time is 1 hour, so that the cured carbon fiber felt is obtained.
As shown in Table 1, the cured carbon fiber felt prepared in this example had a density of 3.4g/cm 3 The thermal conductivity coefficient is 1.6W/mk, the ash content is 378ppm, and the specific heat is 2.6J/g.k.
This comparative example illustrates that without the foaming process, the density in the cured carbon fiber mat is higher, the carbon fibers are not sufficiently dispersed, and the thermal properties are also poor.
TABLE 1 Properties of the cured carbon fiber felts prepared in examples 1 to 5 and comparative examples 1 to 3
Claims (8)
1. A preparation method of a solidified carbon fiber felt is characterized by comprising the following steps: the method comprises the following steps:
1) Stirring and mixing a mixture A consisting of polyether propylene glycol, polyether glycerol and carbon fibers, a mixture B consisting of liquid resin, an organic solvent and carbon fibers and a mixture C consisting of polymethylene polyphenyl polyisocyanate, the organic solvent and the carbon fibers, and performing prepolymerization reaction to obtain a prepolymer;
2) Transferring the prepolymer into a mold for foaming and curing to obtain a cured carbon fiber felt precursor;
3) Carbonizing and graphite treating the cured carbon fiber precursor to obtain a cured carbon fiber felt;
the mixing mass ratio of the mixture A to the mixture B to the mixture C is 1:1 to 1.4:1.05 to 1.85;
the liquid resin is at least one of phenolic resin, furan resin, epoxy resin, polyamide resin, urea resin and polyurethane resin;
the mixture A consists of polyether propylene glycol, polyether glycerol and carbon fiber in a mass ratio of 1-2;
the organic solvent is at least one of absolute alcohol, acetone, isopropanol, diethyl ether and propylene oxide.
2. The method of producing a cured carbon fiber mat according to claim 1, wherein: the water mass fraction of the mixture A is less than or equal to 5 percent, and the pH value is 5.5-7.5.
3. The method of claim 1, wherein the carbon fiber mat is prepared by: the mixture B consists of liquid resin, an organic solvent and carbon fiber according to a mass ratio of 4.
4. The method of claim 1, wherein the carbon fiber mat is prepared by: the mixture C comprises polymethylene polyphenyl polyisocyanate, an organic solvent and carbon fibers according to the mass ratio of 2-5.
5. The method for producing a cured carbon fiber mat according to any one of claims 1 to 4, wherein:
the temperature of the prepolymerization reaction is 15-95 ℃, and the time is 10-60 minutes;
the foaming and curing time is 20-120 minutes.
6. The method for producing a cured carbon fiber mat according to any one of claims 1 to 4, characterized in that: the carbonization temperature is 500-1100 ℃, and the time is 1-3 hours;
the graphitization temperature is 1800-2400 ℃, and the time is 1-3 hours.
7. A cured carbon fiber mat characterized by: the method according to any one of claims 1 to 6.
8. The cured carbon fiber mat according to claim 7, wherein: the density of the solidified carbon fiber felt is 0.18g/cm 3 ～0.22g/cm 3 The heat conductivity coefficient is 0.19W/mk-0.22W/mk, the ash content is less than or equal to 28ppm, and the specific heat is 0.35J/g.k-0.65J/g.k.
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