CN115816925A - Graphene nanosheet-based modified carbon fiber composite material and preparation method thereof - Google Patents
Graphene nanosheet-based modified carbon fiber composite material and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of composite material manufacturing, and particularly relates to a graphene nanosheet modified carbon fiber composite material and a preparation method thereof. The preparation method of the material comprises the following steps: preparing a polyelectrolyte aqueous solution, adding graphene nanosheets, and preparing a graphene dispersion solution through ultrasonic dispersion; pouring the graphene dispersion liquid on the surface of the flat carbon fiber cloth, wetting the carbon fiber cloth, alternately laying and wetting until the carbon fiber cloth is laid in a laminated manner to 5-30 layers, and drying and carrying out high-temperature heat treatment to obtain a prefabricated body; and preparing a resin glue solution, impregnating the prefabricated body with the resin glue solution by adopting a vacuum infusion process, and heating and curing to obtain the graphene nanosheet modified carbon fiber composite material. The preparation method is simple, the dispersion of graphene can be avoided, and the bending strength, the bending modulus, the interlaminar shear strength, the heat conduction performance and the electric conduction performance of the obtained composite material are obviously improved.
Description
Technical Field
The invention belongs to the technical field of composite material manufacturing, and particularly relates to a graphene nanosheet modified carbon fiber composite material and a preparation method thereof.
Background
The carbon fiber reinforced resin matrix Composite (CFRP) is widely applied to the fields of aerospace, transportation, equipment manufacturing and the like due to the advantages of light weight, high strength, good fatigue resistance, simple preparation process and the like. Due to the anisotropy of the carbon fiber material, the carbon fiber composite material has excellent longitudinal mechanical, thermal and electrical properties, but has lower mechanical properties in the transverse direction. Meanwhile, because the fiber cloth is bonded by matrix resin, the transverse heat conduction and the electric conduction of the composite material are poor, and the application range of the carbon fiber composite material is limited.
With the rapid development of nanotechnology, the nanomaterial-modified carbon fiber composite material attracts people's extensive attention. Due to the unique geometric structure, graphene has unique mechanical, optical, electromagnetic and other properties, which arouses research interest. The graphene is considered as the optimal two-dimensional nano modified material of the polymer, and the mechanical property, the thermal property, the electrical property and the like of the composite material can be further improved by introducing the fiber reinforced resin matrix composite material into the graphene. The traditional preparation method of the nano-material modified carbon fiber composite material generally comprises the steps of dispersing graphene in an organic solvent, adding a resin glue solution, and compounding a graphene/resin glue solution mixture and fibers by a proper method to prepare the graphene modified carbon fiber composite material. The traditional preparation method usually uses an organic solvent, and graphene is easily filtered by fibers when a perfusion process is adopted, so that the graphene is unevenly distributed, and the overall performance of the composite material is influenced. Therefore, the introduction mode of graphene needs to be improved, so that the graphene is introduced into the fiber composite material by an environment-friendly method, and the graphene modified carbon fiber composite material with better performance is prepared.
Disclosure of Invention
The invention aims to provide a graphene nanosheet-based modified carbon fiber composite material and a preparation method thereof.
In order to achieve the purpose, the invention provides the following technical scheme:
the invention provides a preparation method of a graphene nanosheet-based modified carbon fiber composite material, which comprises the following steps:
s1, adding polymer electrolyte into water, heating in a water bath and stirring until the polymer electrolyte is completely dissolved to form a polyelectrolyte aqueous solution;
s2, adding graphene nanosheets into the polyelectrolyte aqueous solution obtained in the step S1, and performing ultrasonic dispersion to prepare a graphene dispersion solution;
s3, pouring the graphene dispersion liquid on the surface of the flat carbon fiber cloth in the step S2 to wet the carbon fiber cloth, laying a layer of carbon fiber cloth, alternately pouring the graphene dispersion liquid and laying the carbon fiber cloth until the carbon fiber cloth is laminated and laid for 5-30 layers, and drying and carrying out high-temperature heat treatment to obtain a graphene/carbon fiber composite prefabricated body;
s4, preparing a resin glue solution, impregnating the graphene/carbon fiber composite prefabricated body in the step S3 with the resin glue solution by adopting a vacuum infusion process, and heating and curing to obtain the graphene nanosheet modified carbon fiber composite material.
The polymer electrolyte in the present invention functions to disperse graphene.
Preferably, the polymer electrolyte in step S1 is polyvinyl alcohol, and the weight average molecular weight of the polyvinyl alcohol is 2.5 to 15 ten thousand.
Preferably, the water bath heating temperature in the step S1 is 85-100 ℃, the stirring mode is magnetic stirring or mechanical stirring, and the stirring speed is 300-1000 rpm.
Preferably, the concentration of the polyelectrolyte aqueous solution in the step S1 is 0.5-2 mg/ml.
Preferably, the graphene nanoplatelets in step S2 are single-layer, double-layer or multi-layer graphene, the thickness of the graphene nanoplatelets is 0.3-25 nm, the radial width is 1-40 μm, the longitudinal thermal conductivity is 1500-3000W/(m · K), and the specific surface area is 10-300 m 2 /g。
Preferably, the power of ultrasonic dispersion in step S2 is 80-700W, and the ultrasonic time is 5-15 min.
Preferably, the concentration of graphene in the graphene dispersion liquid in the step S2 is 0.2 to 4 mg/ml.
Preferably, the drying manner in the step S3 is supercritical drying, the temperature of the high-temperature heat treatment is 650-800 ℃, the time of the high-temperature heat treatment is 1-3 hours, and the atmosphere of the high-temperature heat treatment is high-purity argon or nitrogen.
Preferably, the carbon fiber cloth in step S3 is polyacrylonitrile-based carbon fiber, pitch-based carbon fiber or viscose-based carbon fiber.
Preferably, the mass fraction of graphene in the graphene/carbon fiber composite preform in the step S3 is 0.1 to 3.0 wt.%.
After the high temperature heat treatment of step S3, the polyvinyl alcohol is completely decomposed.
Preferably, the resin glue solution in the step S4 is a mixed glue solution of epoxy resin and an amine curing agent, and the viscosity of the epoxy resin is 600 to 2500 mPa · S; the epoxy resin is low-viscosity bisphenol A epoxy resin, bisphenol F epoxy resin or alicyclic epoxy resin.
More preferably, the mass ratio of the epoxy resin to the amine curing agent in the resin glue solution is (2-6) to 1.
Preferably, in the graphene nanosheet modified carbon fiber composite material based on step S4, the mass fraction of graphene is 0.05 to 1.0 wt.%.
The invention also provides the graphene nanosheet modified carbon fiber composite material prepared by the method.
Compared with the prior art, the preparation method of the graphene nanosheet-based modified carbon fiber composite material has the following outstanding beneficial effects:
(1) According to the invention, the graphene nanosheets are directly combined with the carbon fiber cloth by a supercritical drying method to form a composite preform, the whole composite preform is used as a reinforcing material to prepare the graphene nanosheet modified carbon fiber composite material, and the problem that the graphene nanosheets are difficult to disperse uniformly in the carbon fiber composite material is solved.
(2) The preparation process of the invention does not use organic solvent, thus being green and environment-friendly; the preparation method is simple, and the prepared graphene nanosheet/carbon fiber composite prefabricated body reinforcing material can adapt to a mature vacuum infusion process and can realize large-scale production.
(3) The graphene in the graphene/carbon fiber composite prefabricated body is uniformly distributed among the layers of the fiber cloth and among the fiber gaps, so that the comprehensive performance of the fiber composite material can be obviously enhanced; the bending strength, the bending modulus, the interlaminar shear strength, the heat conduction and the electric conduction performance of the prepared composite material are obviously improved.
Drawings
Fig. 1 is an appearance picture of a graphene/carbon fiber composite preform prepared in example 3 of the present invention.
Fig. 2 is an SEM picture of the graphene/carbon fiber composite preform prepared in example 3 of the present invention.
Detailed Description
The invention will be further described with reference to specific embodiments, and the advantages and features of the invention will become apparent as the description proceeds. The examples are illustrative only and do not limit the scope of the present invention in any way. It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention, and that such changes and modifications may be made without departing from the spirit and scope of the invention.
Example 1
A preparation method of a graphene nanosheet-based modified carbon fiber composite material comprises the following steps:
(1) Adding 0.2 g of polyvinyl alcohol (Mw = 47000) into 200 ml of water, heating in a water bath at 95 ℃, and magnetically stirring at the rotating speed of 500 r/min until the polyvinyl alcohol is completely dissolved to form a polyvinyl alcohol aqueous solution with the concentration of 1 mg/ml;
(2) 0.1 g of multilayer graphene nanosheets (average thickness of 5 nm, average radial width of 5 μm, longitudinal thermal conductivity of 3000W/(m.K), transverse thermal conductivity of 6W/(m.K), specific surface area of 120 m 2 Per gram) is added into 200 ml of polyvinyl alcohol aqueous solution, and ultrasonic dispersion is carried out for 5 min under the power of 250W, thus preparing 0.5 mg/ml graphene dispersion liquid;
(3) 16.6 ml of graphene dispersion liquid is measured and poured into a flat piece of polyacrylonitrile-based unidirectional carbon fiber cloth (24K, 200 g/m) 2 ) Wetting carbon fiber cloth on the surface, laying a layer of carbon fiber cloth, pouring graphene dispersion liquid and laying the carbon fiber cloth alternately until the carbon fiber cloth is laid into 12 layers in a laminated manner, and performing supercritical drying and 700 ℃ heat treatmentProcessing for 2 h to obtain a graphene/carbon fiber composite prefabricated body; the mass fraction of graphene in the composite preform was 0.32 wt.%.
(4) Preparing a mixed glue solution of alicyclic epoxy resin TDE-85 (the room temperature viscosity is 1600-2000 mPa · s) and m-phenylenediamine according to the mass ratio of 100:26.4, impregnating the graphene/carbon fiber composite preform in the step (3) with the glue solution by adopting a vacuum infusion process, and respectively curing for 2 h and 4 h at 80 ℃ and 120 ℃ to obtain the graphene nanosheet modified carbon fiber composite material with the graphene nanosheet content of 0.1 wt.%.
Example 2
A preparation method of a graphene nanosheet-based modified carbon fiber composite material comprises the following steps:
(1) Adding 0.2 g of polyvinyl alcohol (Mw = 47000) into 200 ml of water, heating in a water bath at 95 ℃, and magnetically stirring at the rotating speed of 500 r/min until the polyvinyl alcohol is completely dissolved to form a polyvinyl alcohol aqueous solution with the concentration of 1 mg/ml;
(2) 0.2 g of multilayer graphene nanosheets (average thickness of 5 nm, average radial width of 5 μm, longitudinal thermal conductivity of 3000W/(m.K), transverse thermal conductivity of 6W/(m.K), specific surface area of 120 m 2 Per gram) is added into 200 ml of polyvinyl alcohol aqueous solution, and ultrasonic dispersion is carried out for 5 min under the power of 250W, so as to prepare 1.0 mg/ml of graphene dispersion liquid;
(3) 16.6 ml of graphene dispersion liquid is measured and poured into a flat piece of polyacrylonitrile-based unidirectional carbon fiber cloth (24K, 200 g/m) 2 ) Wetting carbon fiber cloth on the surface, laying a layer of carbon fiber cloth, pouring graphene dispersion liquid and laying the carbon fiber cloth alternately until the carbon fiber cloth is laid to 12 layers in a laminated manner, and carrying out supercritical drying and heat treatment at 700 ℃ for 2 hours to obtain a graphene/carbon fiber composite preform; the mass fraction of graphene in the composite preform was 0.64 wt.%.
(4) Preparing a mixed glue solution of alicyclic epoxy resin TDE-85 (the room temperature viscosity is 1600-2000 mPa · s) and m-phenylenediamine according to the mass ratio of 100.4, impregnating the graphene/carbon fiber composite preform in the step (3) with the glue solution by adopting a vacuum infusion process, and respectively curing for 2 h and 4 h at 80 ℃ and 120 ℃ to obtain the graphene nanosheet modified carbon fiber composite material with the graphene nanosheet content of 0.2 wt.%.
Example 3
A preparation method of a graphene nanosheet-based modified carbon fiber composite material comprises the following steps:
(1) Adding 0.2 g of polyvinyl alcohol (Mw = 47000) into 200 ml of water, heating in a water bath at 95 ℃, and magnetically stirring at the rotating speed of 500 r/min until the polyvinyl alcohol is completely dissolved to form a polyvinyl alcohol aqueous solution with the concentration of 1 mg/ml;
(2) 0.3 g of multilayer graphene nanosheets (average thickness of 5 nm, average radial width of 5 μm, longitudinal thermal conductivity of 3000W/(m.K), transverse thermal conductivity of 6W/(m.K), specific surface area of 120 m 2 Per gram) is added into 200 ml of polyvinyl alcohol aqueous solution, and ultrasonic dispersion is carried out for 5 min under the power of 250W to prepare 1.5 mg/ml of graphene dispersion liquid;
(3) 16.6 ml of graphene dispersion liquid is measured and poured into a flat piece of polyacrylonitrile-based unidirectional carbon fiber cloth (24K, 200 g/m) 2 ) Wetting carbon fiber cloth on the surface, laying a layer of carbon fiber cloth, pouring graphene dispersion liquid and laying the carbon fiber cloth alternately until the carbon fiber cloth is layered and laid to 12 layers, and performing supercritical drying and 700 ℃ heat treatment for 2 hours to obtain a graphene/carbon fiber composite preform; the mass fraction of graphene in the composite preform was 0.96 wt.%.
(4) Preparing a mixed glue solution of alicyclic epoxy resin TDE-85 (the room temperature viscosity is 1600-2000 mPa · s) and m-phenylenediamine according to the mass ratio of 100.4, impregnating the graphene/carbon fiber composite preform in the step (3) with the glue solution by adopting a vacuum infusion process, and respectively curing for 2 h and 4 h at 80 ℃ and 120 ℃ to obtain the graphene nanosheet modified carbon fiber composite material with the graphene nanosheet content of 0.3 wt.%.
Example 4
A preparation method of a graphene nanosheet-based modified carbon fiber composite material comprises the following steps:
(1) Adding 0.2 g of polyvinyl alcohol (Mw = 47000) into 200 ml of water, heating in a water bath at 95 ℃, and magnetically stirring at the rotating speed of 500 r/min until the polyvinyl alcohol is completely dissolved to form a polyvinyl alcohol aqueous solution with the concentration of 1 mg/ml;
(2) 0.4 g of multilayer graphene nanosheets (average thickness of 5 nm, average radial width of 5 μm, longitudinal thermal conductivity of 3000W/(m.K), transverse thermal conductivity of 6W/(m.K), specific surface area of 120 m 2 Adding the mixture into 200 ml of polyvinyl alcohol aqueous solution, and ultrasonically dispersing for 5 min under the power of 250W to prepare 2 mg/ml graphene dispersion liquid;
(3) 16.6 ml of graphene dispersion liquid is measured and poured into a piece of flat polyacrylonitrile-based unidirectional carbon fiber cloth (24K, 200 g/m) 2 ) Wetting carbon fiber cloth on the surface, laying a layer of carbon fiber cloth, pouring graphene dispersion liquid and laying the carbon fiber cloth alternately until the carbon fiber cloth is laid to 12 layers in a laminated manner, and carrying out supercritical drying and heat treatment at 700 ℃ for 2 hours to obtain a graphene/carbon fiber composite preform; the mass fraction of graphene in the composite preform was 1.28 wt.%.
(4) Preparing a mixed glue solution of alicyclic epoxy resin TDE-85 (the room temperature viscosity is 1600-2000 mPa · s) and m-phenylenediamine according to the mass ratio of 100.4, impregnating the graphene/carbon fiber composite preform in the step (3) with the glue solution by adopting a vacuum infusion process, and respectively curing for 2 h and 4 h at 80 ℃ and 120 ℃ to obtain the graphene nanosheet modified carbon fiber composite material with the graphene nanosheet content of 0.4 wt.%.
Comparative example 1
A preparation method of a carbon fiber composite material comprises the following steps:
(1) Adding 0.2 g of polyvinyl alcohol (Mw = 47000) into 200 ml of water, heating and stirring in a water bath at 95 ℃ until the polyvinyl alcohol is completely dissolved to form a polyvinyl alcohol aqueous solution with the concentration of 1 mg/ml;
(2) 16.6 ml of polyvinyl alcohol aqueous solution is measured and poured into a flat piece of polyacrylonitrile-based unidirectional carbon fiber cloth (24K, 200 g/m) 2 ) Wetting carbon fiber cloth on the surface, laying a layer of carbon fiber cloth, pouring polyvinyl alcohol aqueous solution and laying the carbon fiber cloth alternately until the carbon fiber cloth is laid to 12 layers in a laminated manner, and carrying out supercritical drying and 700 ℃ heat treatment for 2 hours to obtain a carbon fiber composite preform;
(3) Preparing a mixed glue solution of alicyclic epoxy resin TDE-85 and m-phenylenediamine according to the mass ratio of 100.4, impregnating the carbon fiber composite preform in the step (3) with the glue solution by adopting a vacuum infusion process, and respectively curing for 2 h and 4 h at 80 ℃ and 120 ℃ to obtain an unmodified carbon fiber composite material; wherein the volume fraction of carbon fibers in the carbon fiber composite material is 72 vol.%.
Comparative example 2
A carbon fiber composite material preparation method, which is different from that of example 1 in that the graphene mass fraction in the graphene/carbon fiber composite preform of step (3) is 3.8 wt.%; and the mass fraction of graphene in the finally obtained graphene nanosheet modified carbon fiber composite material is 1.2 wt.%.
Characterization and results of Performance
The specimens obtained in examples 1 to 4 and comparative examples 1 to 2 were subjected to flexural strength test in accordance with ASTM D790, interlaminar shear strength test in accordance with ASTM D2344, thermal conductivity test in accordance with ASTM-E1461, and volume resistivity test in accordance with ASTM D257, and the test results are shown in Table 1.
Table 1 shows performance test results of graphene nanosheet modified carbon fiber composite materials obtained in examples and comparative examples
It can be seen that, compared with comparative example 1, in examples 1 to 4 of the present invention, as the content of the graphene nanosheet in the prepared graphene/carbon fiber/epoxy resin composite material increases, the bending strength, the bending modulus, the interlaminar shear strength and the thermal conductivity of the composite material are significantly improved, and the volume resistivity is reduced. The graphene/carbon fiber composite prefabricated body can be completely infiltrated by resin within a proper graphene content range, the graphene has good dispersibility in the carbon fiber composite material (see the attached figures 1 and 2 in the specification), an effective heat conduction and electric conduction network is formed between the layers of the composite material, the modification effect of the graphene is fully exerted, and the mechanics, heat conduction and electric conduction performance of the composite material are improved.
Comparative example 2 shows that: when the content of graphene in the carbon fiber composite material exceeds 1.0 wt.%, the mechanical properties of the composite material, such as flexural strength, flexural modulus and interlaminar shear strength, are lower than those of examples 1 to 4, the thermal conductivity is lower than those of examples 3 and 4, and the volume resistivity is higher than those of examples 3 and 4. The reason is that when the content of graphene in the carbon fiber composite material is too high, the graphene is not uniformly distributed, and the graphene/carbon fiber composite preform is more compact, so that the graphene/carbon fiber composite preform cannot be fully impregnated by glue solution, and the composite material has more defects.
According to the technology, a proper amount of graphene nanosheets are directly combined with the carbon fiber cloth through a supercritical drying method to form a composite prefabricated body, the high-performance graphene nanosheet modified carbon fiber composite material can be prepared in batches through a vacuum infusion process, and the preparation process is environment-friendly.
Claims (10)
1. A preparation method of a graphene nanosheet-based modified carbon fiber composite material is characterized by comprising the following steps:
s1, adding polymer electrolyte into water, heating in a water bath and stirring until the polymer electrolyte is completely dissolved to form a polyelectrolyte aqueous solution;
s2, adding graphene nanosheets into the polyelectrolyte aqueous solution obtained in the step S1, and performing ultrasonic dispersion to prepare a graphene dispersion solution;
s3, pouring the graphene dispersion liquid on the surface of the flat carbon fiber cloth in the step S2 to wet the carbon fiber cloth, laying a layer of carbon fiber cloth, alternately pouring the graphene dispersion liquid and laying the carbon fiber cloth until the carbon fiber cloth is laminated and laid for 5-30 layers, and drying and carrying out high-temperature heat treatment to obtain a graphene/carbon fiber composite prefabricated body;
s4, preparing a resin glue solution, impregnating the graphene/carbon fiber composite prefabricated body in the step S3 with the resin glue solution by adopting a vacuum infusion process, and heating and curing to obtain the graphene nanosheet modified carbon fiber composite material.
2. The method according to claim 1, wherein the polymer electrolyte in step S1 is polyvinyl alcohol having a weight average molecular weight of 2.5 to 15 ten thousand; preferably, the water bath heating temperature in the step S1 is 85-100 ℃, the stirring mode is magnetic stirring or mechanical stirring, and the stirring speed is 300-1000 rpm.
3. The method according to claim 1, wherein the concentration of the aqueous polyelectrolyte solution in step S1 is 0.5 to 2 mg/ml.
4. The preparation method according to claim 1, wherein the graphene nanoplatelets in step S2 are single-layer, double-layer or multi-layer graphene, the graphene nanoplatelets have a thickness of 0.3 to 25 nm, a radial width of 1 to 40 μm, a longitudinal thermal conductivity of 1500 to 3000W/(m-K), and a specific surface area of 10 to 300 m 2 (ii)/g; preferably, the power of ultrasonic dispersion in step S2 is 80-700W, and the ultrasonic time is 5-15 min.
5. The method according to claim 1, wherein the concentration of graphene in the graphene dispersion liquid in step S2 is 0.2 to 4 mg/ml.
6. The preparation method according to claim 1, wherein the drying manner in step S3 is supercritical drying, the temperature of the high-temperature heat treatment is 650 to 800 ℃, the time of the high-temperature heat treatment is 1 to 3 hours, and the atmosphere of the high-temperature heat treatment is high-purity argon or nitrogen; preferably, the carbon fiber cloth in the step S3 is polyacrylonitrile-based carbon fiber, pitch-based carbon fiber or viscose-based carbon fiber; preferably, the mass fraction of graphene in the graphene/carbon fiber composite preform in the step S3 is 0.1 to 3.0 wt.%.
7. The preparation method according to claim 1, wherein the resin glue solution in the step S4 is a mixed glue solution of epoxy resin and amine curing agent, and the viscosity of the epoxy resin is 600 to 2500 mPa-S; the epoxy resin is low-viscosity bisphenol A epoxy resin, bisphenol F epoxy resin or alicyclic epoxy resin.
8. The preparation method according to claim 7, wherein the mass ratio of the epoxy resin to the amine curing agent in the resin glue solution is (2-6): 1.
9. The preparation method according to claim 1, wherein the mass fraction of graphene in the graphene nanoplatelet-based modified carbon fiber composite material of step S4 is 0.05 to 1.0 wt.%.
10. Graphene nanoplatelet-based modified carbon fiber composite prepared according to the preparation method of any one of claims 1 to 9.
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