CN115028466B - Carbon fiber composite material and preparation method thereof - Google Patents
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Abstract
The application relates to the technical field of carbon fiber materials, and particularly discloses a carbon fiber composite material and a preparation method thereof. The carbon fiber composite material is prepared by polymerizing the following raw materials in parts by weight: 90-95 parts of carbon fiber felt; 75-80 parts of phenolic resin; 20-25 parts of polyethylene resin; 1-2 parts of a flame retardant; 1-2 parts of a crosslinking agent; 0.8-1 part of fumed silica; 2-2.5 parts of modified alumina; 30-35 parts of silicon carbide; the preparation method comprises the following steps: soaking the carbon fiber felt in a nitric acid solution, taking out, drying and activating; stirring and mixing the rest raw materials to obtain composite resin; pouring 2/3 of composite resin on the activated carbon fiber felt, and performing hot-pressing to obtain a primary material; and stirring and mixing 1/3 of the composite resin and silicon carbide, brushing the mixture on the upper surface and the lower surface of the primary material, placing the mixture in a graphitization furnace for graphitization treatment, and cooling to obtain the carbon fiber composite material. The carbon fiber composite material is a high-temperature fire-resistant heat-insulating material and has the advantages of good compressive strength and low density.
Description
Technical Field
The application relates to the technical field of carbon fiber materials, in particular to a carbon fiber composite material and a preparation method thereof.
Background
Carbon fiber is a reinforced material developed after the 50 s of the 20 th century, has excellent properties of high specific strength, high specific modulus, high temperature resistance, corrosion resistance, electric conductivity, small thermal expansion coefficient and the like, and is widely applied to the fields of aerospace, sports equipment and the like.
A high-performance carbon fiber composite heat-insulating material is a high-temperature fire-resistant heat-insulating material, which is a high-temperature heat-insulating material with density gradient and is obtained by compounding a high-temperature-resistant carbon fiber heat-insulating felt with anisotropic fiber orientation and phenolic resin and then graphitizing, has the excellent characteristics of light weight, high strength, wear resistance, high temperature resistance, high conductivity and the like, is mainly used in high-temperature vacuum equipment, and is widely applied to the fields of metal heat treatment, sintering of fine ceramics, generation of various crystals, production of optical fibers, sintering of silicon substrates and semiconductor monocrystalline silicon used in solar power generation systems and the like.
The performance of the carbon fiber composite material depends on the performance of a matrix material, the bonding degree of fibers and the matrix material and the like, the surface is studied, the active specific surface area of the carbon fibers is small before surface treatment, the surface energy is low, the surface is lyophobic, and the fiber surface treatment is to enhance the chemical activity and the physical activity of the fiber surface so as to increase the bonding or adhesion between the fiber surface and the matrix. However, in the research of commonly treating the surface of the fiber to increase the cohesiveness of the composite material, the method of surface oxidation of the fiber is mainly used, and after the surface oxidation of the fiber, the prepared carbon fiber composite material has high density, low compressive strength and limited applicability.
Disclosure of Invention
In order to improve the compressive strength of the carbon fiber composite material and reduce the density of the carbon fiber composite material, the application provides the carbon fiber composite material and the preparation method thereof.
In a first aspect, the present application provides a carbon fiber composite material, which adopts the following technical scheme:
the carbon fiber composite material is prepared by polymerizing the following raw materials in parts by weight: 90-95 parts of carbon fiber felt; 75-80 parts of phenolic resin; 20-25 parts of polyethylene resin; 1-2 parts of a flame retardant; 1-2 parts of a crosslinking agent; 0.8-1 part of fumed silica; 2-2.5 parts of modified alumina; 30-35 parts of silicon carbide.
According to the technical scheme, the carbon fiber felt is made of the base material and has a large specific surface area and good high-temperature resistance, the phenolic resin and the polyethylene resin are mixed and then added with the cross-linking agent, so that the phenolic resin and the cross-linking agent can generate cross-linking reaction, the performance of a resin mixture is improved, the flame retardant, the fumed silica, the modified alumina, the silicon carbide and the resin mixture are mixed, the flame retardant, the fumed silica, the modified alumina, the modified silicon carbide and the resin mixture can improve the flame retardant performance and the structural strength of the resin mixture, the modified alumina can be better distributed in the resin mixture through modification, the structural strength and the compressive strength of the whole body can be improved through the modified alumina, and the compressive strength of the whole body can be further enhanced through the silicon carbide; and mixing the carbon fiber felt with the resin mixture, so that the resin mixture permeates into the carbon fiber felt and is pressed, and graphitizing to obtain the carbon fiber composite material with high compressive strength and low density.
Preferably, the modified alumina is prepared by the following steps: ball milling alumina, sieving with 500 mesh sieve, adding into ethanol, ultrasonic oscillating for 30min, filtering, and oven drying; and (2) activating the dried alumina powder in an environment of 80 ℃ for 1h, adding the activated alumina powder into an ethyl acetate solution, stirring, adding a silane coupling agent and formic acid, stirring and mixing for 1h, filtering and drying to obtain the modified alumina.
Preferably, the weight part ratio of the alumina powder to the silane coupling agent to the formic acid is (2-2.5): (0.2-0.3): (0.1-0.15).
Preferably, the silane coupling agent is dimethyldiethoxysilane.
Preferably, the crosslinking agent is cashew alcohol.
Preferably, the carbon fiber felt has a thickness of 5 to 15mm.
Preferably, the flame retardant is mica powder, and the mesh number of the mica powder is 1000-2000 meshes.
In a second aspect, the present application provides a method for preparing a carbon fiber composite material, which adopts the following technical scheme:
the preparation method of the carbon fiber composite material comprises the following steps: placing the carbon fiber felt in a nitric acid solution for soaking for 1h, taking out and drying the carbon fiber felt, and placing the carbon fiber felt in a nitrogen environment at 100 ℃ for activation for later use; stirring and mixing phenolic resin, polyethylene resin and a cross-linking agent, sequentially adding a flame retardant, fumed silica and modified alumina, and stirring and mixing to obtain composite resin; pouring 2/3 of the composite resin on the activated carbon fiber felt, and performing hot pressing at 90-180 ℃ to obtain a primary material; and stirring and mixing 1/3 of the composite resin and silicon carbide, brushing the mixture on the upper surface and the lower surface of the primary material, placing the primary material in a graphitization furnace at 2400 ℃ for heat preservation for 2 hours, and cooling to obtain the carbon fiber composite material.
Preferably, during hot-pressing, the temperature is raised at 90-140 ℃ at 30 ℃/h, the temperature is kept at 140 ℃ for 1h, the temperature is kept at 140-180 ℃ for vertical rising, the temperature is kept at 180 ℃ for 3h, and then the primary material is obtained after cooling.
Preferably, the pressure in the graphitization furnace is 7000-8000Pa.
In summary, the present application has the following beneficial effects: the carbon fiber composite material is prepared by polymerizing the following raw materials in parts by weight: 90-95 parts of carbon fiber felt; 75-80 parts of phenolic resin; 20-25 parts of polyethylene resin; 1-2 parts of a flame retardant; 1-2 parts of a crosslinking agent; 0.8-1 part of fumed silica; 2-2.5 parts of modified alumina; 30-35 parts of silicon carbide; the carbon fiber felt is composed of a base material and has a large specific surface area and good high-temperature resistance, the phenolic resin and the polyethylene resin are mixed and then added with the cross-linking agent, so that the phenolic resin and the cross-linking agent can generate a cross-linking reaction, the performance of a resin mixture is improved, the flame retardant, the fumed silica, the modified alumina, the silicon carbide and the resin mixture are mixed, the flame retardant and the structural strength of the resin mixture can be improved, the modified alumina can be better distributed in the resin mixture after modification treatment, the overall structural strength and compressive strength of the modified alumina can be improved, and the overall compressive strength of the silicon carbide can be further enhanced; and mixing the carbon fiber felt with the resin mixture, so that the resin mixture permeates into the carbon fiber felt and is pressed, and graphitizing to obtain the carbon fiber composite material with high compressive strength and low density.
Detailed Description
The present application will be described in further detail below with reference to examples 1 to 3 and comparative examples 1 to 4.
Examples
Examples 1 to 3
The weight parts of each raw material of the carbon fiber composite materials in examples 1 to 3 are shown in table 1.
TABLE 1 parts by weight of carbon fiber composite feedstock in examples 1-3
| Example 1 | Example 2 | Example 3 | |
| Carbon fiber felt | 90 | 95 | 93 |
| Phenolic resin | 75 | 80 | 77 |
| Polyethylene resin | 20 | 25 | 23 |
| Flame retardant | 1 | 2 | 1.5 |
| Crosslinking agent | 1 | 2 | 1.3 |
| Fumed silica | 0.8 | 1 | 0.9 |
| Modified alumina | 2 | 2.5 | 2.2 |
| Silicon carbide | 30 | 35 | 33 |
In the present examples 1 to 3, the carbon fiber felt had a thickness of 5 to 15mm, the flame retardant was mica powder having a mesh number of 1000 to 2000, the crosslinking agent was cashew alcohol, and the silicon carbide had a mesh number of 500 to 1000.
In examples 1-3, modified alumina was prepared by the following steps: ball-milling alumina, sieving with 500 mesh sieve, adding into ethanol, ultrasonic vibrating for 30min, filtering, and oven drying; activating the dried alumina powder in an environment of 80 ℃ for 1 hour, adding the activated alumina powder into an ethyl acetate solution, stirring, adding a silane coupling agent and formic acid, stirring and mixing for 1 hour, filtering and drying to obtain modified alumina; wherein the weight part ratio of the alumina powder to the silane coupling agent to the formic acid is (2-2.5): (0.2-0.3): (0.1-0.15); specifically, the silane coupling agent was dimethyldiethoxysilane, and in example 1, the weight part of the silane coupling agent was 0.2 and the weight part of formic acid was 0.1, in example 2, the weight part of the silane coupling agent was 0.3 and the weight part of formic acid was 0.15, in example 3, the weight part of the silane coupling agent was 0.3 and the weight part of formic acid was 0.13.
The preparation method of the carbon fiber composite material in the embodiments 1 to 3 includes the following steps: soaking the carbon fiber felt in a nitric acid solution for 1 hour, taking out, drying, and activating in a nitrogen environment at 100 ℃ for later use; stirring and mixing phenolic resin, polyethylene resin and a cross-linking agent, sequentially adding a flame retardant, fumed silica and modified alumina, and stirring and mixing to obtain composite resin; pouring 2/3 of the composite resin on the activated carbon fiber felt, placing the carbon fiber felt in a hot press, performing hot pressing at the temperature of 90-180 ℃, wherein the temperature of 90-140 ℃ is raised by 30 ℃/h, preserving heat at 140 ℃ for 1h, preserving heat at 140-180 ℃ for 3h, and cooling to obtain a primary material; stirring and mixing 1/3 of the composite resin and silicon carbide, brushing the mixture on the upper surface and the lower surface of the primary material, keeping the temperature of the brushed carbon fiber felt in a graphitization furnace at 2400 ℃ and the pressure of 7000-8000Pa for 2 hours, and cooling to obtain the carbon fiber composite material, wherein the brushing thickness is 2-3 mm.
Through measurement:
the bulk density of the carbon fiber composite in example 1 was 0.205g/cm 3 Compressive strength of 0.89MPa (in the plane direction) and 0.46MPa (in the both-side direction), and bending strength of 4.22MPa (in the plane direction) and 2.48MPa (in the both-side direction);
the bulk density of the carbon fiber composite in example 2 was 0.210g/cm 3 Compressive strength of 0.87MPa (in the plane direction) and 0.45MPa (in the both-side direction), and bending strength of 4.20MPa (in the plane direction) and 2.47MPa (in the both-side direction);
the bulk density of the carbon fiber composite in example 3 was 0.207g/cm 3 The compressive strength was 0.88MPa (in the plane direction) and 0.47MPa (in the both-side direction), and the flexural strength was 4.23MPa (in the plane direction) and 2.49MPa (in the both-side direction).
Comparative example
Comparative example 1
Comparative example 1 is different from example 3 in that the raw material of the carbon fiber composite material in comparative example 1 does not contain the polyethylene resin and the crosslinking agent.
The method for preparing the carbon fiber composite material in comparative example 1 includes the following steps: placing the carbon fiber felt in a nitric acid solution for soaking for 1h, taking out and drying the carbon fiber felt, and placing the carbon fiber felt in a nitrogen environment at 100 ℃ for activation for later use; adding a flame retardant, fumed silica and modified alumina into the phenolic resin in sequence, stirring and mixing to obtain a composite resin; pouring 2/3 of the composite resin on the activated carbon fiber felt, placing the carbon fiber felt in a hot press, performing hot pressing at the temperature of 90-180 ℃, wherein the temperature of 90-140 ℃ is raised by 30 ℃/h, preserving heat at 140 ℃ for 1h, preserving heat at 140-180 ℃ for 3h, and cooling to obtain a primary material; stirring and mixing 1/3 of the composite resin and silicon carbide, brushing the mixture on the upper surface and the lower surface of the primary material, keeping the temperature of the brushed carbon fiber felt in a graphitization furnace at 2400 ℃ and the pressure of 7000-8000Pa for 2 hours, and cooling to obtain the carbon fiber composite material, wherein the brushing thickness is 2-3 mm.
The carbon fiber composite material in comparative example 1 was measured to have a bulk density of 0.184g/cm3, a compressive strength of 0.71MPa (in the in-plane direction) and 0.39MPa (in the both-side direction), and a flexural strength of 3.68MPa (in-plane direction) and 1.89MPa (in the both-side direction).
Comparative example 2
Comparative example 2 differs from example 3 in that the raw material of the carbon fiber composite in comparative example 2 does not contain a crosslinking agent.
The preparation method of the carbon fiber composite material in comparative example 2 comprises the following steps: placing the carbon fiber felt in a nitric acid solution for soaking for 1h, taking out and drying the carbon fiber felt, and placing the carbon fiber felt in a nitrogen environment at 100 ℃ for activation for later use; stirring and mixing phenolic resin and polyethylene resin, sequentially adding a flame retardant, fumed silica and modified alumina, and stirring and mixing to obtain composite resin; pouring 2/3 of the composite resin on the activated carbon fiber felt, placing the carbon fiber felt in a hot press, performing hot pressing at the temperature of 90-180 ℃, heating at the temperature of 90-140 ℃ at 30 ℃/h, preserving heat at the temperature of 140 ℃ for 1h, preserving heat at the temperature of 140-180 ℃ for 3h, and cooling to obtain a primary material; stirring and mixing 1/3 of the composite resin and silicon carbide, brushing the mixture on the upper surface and the lower surface of the primary material, keeping the temperature of the brushed carbon fiber felt in a graphitization furnace at 2400 ℃ and the pressure of 7000-8000Pa for 2 hours, and cooling to obtain the carbon fiber composite material, wherein the brushing thickness is 2-3 mm.
The carbon fiber composite material in comparative example 2 was measured to have a bulk density of 0.204g/cm3, a compressive strength of 0.75MPa (in the plane direction), a compressive strength of 0.42MPa (in the both-side direction), a bending strength of 3.76MPa (in the plane direction), and a bending strength of 1.95MPa (in the both-side direction).
Comparative example 3
Comparative example 3 differs from example 3 in that the raw material of the carbon fiber composite in comparative example 3 does not contain modified alumina.
The preparation method of the carbon fiber composite material in comparative example 3 comprises the following steps: placing the carbon fiber felt in a nitric acid solution for soaking for 1h, taking out and drying the carbon fiber felt, and placing the carbon fiber felt in a nitrogen environment at 100 ℃ for activation for later use; stirring and mixing phenolic resin, polyethylene resin and a cross-linking agent, sequentially adding a flame retardant and gas-phase white carbon black, and stirring and mixing to obtain composite resin; pouring 2/3 of the composite resin on the activated carbon fiber felt, placing the carbon fiber felt in a hot press, performing hot pressing at the temperature of 90-180 ℃, heating at the temperature of 90-140 ℃ at 30 ℃/h, preserving heat at the temperature of 140 ℃ for 1h, preserving heat at the temperature of 140-180 ℃ for 3h, and cooling to obtain a primary material; stirring and mixing 1/3 of the composite resin and silicon carbide, coating the mixture on the upper surface and the lower surface of the primary material, keeping the coating thickness at 2-3mm, placing the coated carbon fiber felt in a graphitization furnace at 2400 ℃ and at the pressure of 7000-8000Pa, preserving the heat for 2h, and cooling to obtain the carbon fiber composite material.
The carbon fiber composite material in comparative example 3 was measured to have a bulk density of 0.174g/cm3, a compressive strength of 0.67MPa (in the in-plane direction), a compressive strength of 0.28MPa (in the both-side direction), a bending strength of 4.02MPa (in-plane direction), and a bending strength of 2.15MPa (in the both-side direction).
Comparative example 4
Comparative example 4 differs from example 3 in that the raw material of the carbon fiber composite material in comparative example 4 does not contain modified alumina and contains 2.2 parts of 500 to 2000 mesh alumina.
The preparation method of the carbon fiber composite material in comparative example 4 comprises the following steps: placing the carbon fiber felt in a nitric acid solution for soaking for 1h, taking out and drying the carbon fiber felt, and placing the carbon fiber felt in a nitrogen environment at 100 ℃ for activation for later use; stirring and mixing phenolic resin, polyethylene resin and a cross-linking agent, sequentially adding a flame retardant, fumed silica and alumina, and stirring and mixing to obtain composite resin; pouring 2/3 of the composite resin on the activated carbon fiber felt, placing the carbon fiber felt in a hot press, performing hot pressing at the temperature of 90-180 ℃, wherein the temperature of 90-140 ℃ is raised by 30 ℃/h, preserving heat at 140 ℃ for 1h, preserving heat at 140-180 ℃ for 3h, and cooling to obtain a primary material; stirring and mixing 1/3 of the composite resin and silicon carbide, coating the mixture on the upper surface and the lower surface of the primary material, keeping the coating thickness at 2-3mm, placing the coated carbon fiber felt in a graphitization furnace at 2400 ℃ and at the pressure of 7000-8000Pa, preserving the heat for 2h, and cooling to obtain the carbon fiber composite material.
As a result of measurement, the carbon fiber composite material in comparative example 4 had a bulk density of 0.208g/cm3, a compressive strength of 0.73MPa (in the plane direction), a compressive strength of 0.34MPa (in the both-side directions), a bending strength of 3.85MPa (in the plane direction), and a bending strength of 2.02MPa (in the both-side directions).
Performance analysis
Combining the measured data of examples 1-3 and the respective data, it can be seen that the carbon fiber composite material of the present application has a lower bulk density, and at the same time, has better compressive strength and bending strength properties.
Combining example 3 and comparative example 1, and combining the respective measurement data, it can be seen that when the polyethylene resin and the crosslinking agent are not added in comparative example 1, the volume density of the carbon fiber composite material obtained by performing hot pressing on the phenolic resin and the carbon fiber composite material is obviously reduced, but the compressive strength and the flexural strength are also obviously reduced. From this fact, it is found that the use of a phenol resin and a polyethylene resin in combination can improve the overall compressive strength and flexural strength, and the effect on the overall performance is not significant although the density is increased.
Combining example 3 and comparative example 2, and combining the respective measurement data, it can be seen that when the phenolic resin and the polyethylene resin are mixed in comparative example 2, but no crosslinking agent is added, so that most of the phenolic resin and the polyethylene resin in the mixed resin exist in the form of monomers, a crosslinking reaction is difficult to occur, and the density of the carbon fiber composite material in comparative example 2 is increased, but the compressive strength and the flexural strength are still inferior to those of the carbon fiber composite material in example 3. From this fact, it is found that the phenolic resin and the polyethylene resin are used in a crosslinked state, and contribute to improvement in the overall compressive strength and flexural strength.
By combining example 3 and comparative example 3, and by combining the respective measurement data, it can be seen that when no modified alumina is added in comparative example 3, the density of the prepared carbon fiber composite material is reduced, the compressive strength performance is also obviously reduced, and the bending strength performance is also reduced in a small degree.
Combining example 3 and comparative example 4, and combining the respective measurement data, it can be seen that when no modified alumina is added in comparative example 4, but alumina is added in the same weight part, the density of the prepared carbon fiber composite material has no obvious change, but the compressive strength and bending strength performance are reduced. It can be seen from the combination of comparative examples 3 and 4 that the distribution is not uniform due to the addition of alumina, resulting in a decrease in the flexural strength.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (7)
1. The carbon fiber composite material is characterized by being prepared from the following raw materials in parts by weight: 90-95 parts of carbon fiber felt; 75-80 parts of phenolic resin; 20-25 parts of polyethylene resin; 1-2 parts of a flame retardant; 1-2 parts of a crosslinking agent; 0.8-1 part of fumed silica; 2-2.5 parts of modified alumina; 30-35 parts of silicon carbide;
the crosslinking agent is cashew alcohol;
the modified alumina is prepared by the following steps: ball milling alumina, sieving with 500 mesh sieve, adding into ethanol, ultrasonic oscillating for 30min, filtering, and oven drying; activating the dried alumina powder in an environment of 80 ℃ for 1 hour, adding the activated alumina powder into an ethyl acetate solution, stirring, adding a silane coupling agent and formic acid, stirring and mixing for 1 hour, filtering and drying to obtain modified alumina;
the preparation method of the carbon fiber composite material comprises the following steps: placing the carbon fiber felt in a nitric acid solution for soaking for 1h, taking out and drying the carbon fiber felt, and placing the carbon fiber felt in a nitrogen environment at 100 ℃ for activation for later use; stirring and mixing phenolic resin, polyethylene resin and a cross-linking agent, sequentially adding a flame retardant, fumed silica and modified alumina, and stirring and mixing to obtain composite resin; 2/3 of the composite resin is poured on the activated carbon fiber felt, and a primary material is obtained after hot pressing and pressing at the temperature of 90-180 ℃; and stirring and mixing 1/3 of the composite resin and silicon carbide, brushing the mixture on the upper surface and the lower surface of the primary material, placing the primary material in a graphitization furnace at 2400 ℃ for heat preservation for 2 hours, and cooling to obtain the carbon fiber composite material.
2. The carbon fiber composite material according to claim 1, characterized in that: the weight part ratio of the alumina powder to the silane coupling agent to the formic acid is (2-2.5): (0.2-0.3): (0.1-0.15).
3. The carbon fiber composite material according to claim 1, characterized in that: the silane coupling agent is dimethyl diethoxy silane.
4. The carbon fiber composite material according to claim 1, characterized in that: the thickness of the carbon fiber felt is 5-15mm.
5. The carbon fiber composite material according to claim 1, characterized in that: the flame retardant is mica powder, and the mesh number of the mica powder is 1000-2000 meshes.
6. The carbon fiber composite material according to claim 1, characterized in that: during hot pressing, the temperature is raised at 90-140 ℃ at 30 ℃/h, the temperature is kept at 140 ℃ for 1h, the temperature is raised at 140-180 ℃ for 3h, and the primary material is obtained after cooling after the temperature is kept at 180 ℃.
7. The carbon fiber composite material according to claim 1, characterized in that: the pressure in the graphitizing furnace is 7000-8000Pa.
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