Preparation method of graphene carbon fiber composite material
By depositing graphene on the surface of carbon fiber and compounding it with epoxy resin, the problem of poor interface performance between carbon fiber and resin matrix was solved, the mechanical properties of the composite material were significantly improved, and the preparation of high-strength and toughness graphene carbon fiber composite materials was achieved.
Patent Information
- Application Number
- CN202510705538.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-05-29
- Publication Date
- 2025-09-16
AI Technical Summary
The poor interface performance between carbon fiber and resin matrix and the brittle resin matrix lead to reduced mechanical properties of composite materials, limiting their application in high-end fields.
The preparation method of graphene-modified composite materials is adopted. By depositing graphene on the surface of carbon fiber and compounding it with epoxy resin, the content of graphene in the composite material is controlled, the complicated dispersion process is avoided, and the interface bonding strength and material properties are improved.
The interfacial shear strength, interlaminar shear strength, flexural strength and impact toughness of the composite material were significantly improved by 67.07%, 64.60%, 32.39% and 41.97% respectively, optimizing the material properties.
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Figure CN120647995A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of material preparation, and in particular to a method for preparing a graphene carbon fiber composite material. Background Art
[0002] Carbon fiber / epoxy resin composite materials have many excellent properties such as light weight, high strength, corrosion resistance, and good designability, and their application fields are becoming more and more extensive. However, due to the poor interface performance between carbon fiber and resin matrix, the brittle resin matrix and other problems, the mechanical properties of the composite materials are reduced, which limits the application of composite materials in high-end fields. In response to this problem, a variety of modification methods have been proposed. Among them, the use of nanoparticles to modify composite materials has become one of the research hotspots in recent years. There are various methods for introducing nanoparticles into carbon fiber composite materials. The present disclosure uses graphene to modify the composite material. Based on this, the present disclosure proposes a method for preparing graphene carbon fiber composite materials. Summary of the Invention
[0003] The present invention provides a method for preparing a graphene-carbon fiber composite material, which effectively controls the graphene content in the composite material while avoiding the complex process of dispersing the graphene in the resin. The method improves the shear strength, flexural strength, and impact toughness of the material.
[0004] According to one aspect of the present disclosure, a method for preparing a graphene carbon fiber composite material is provided, the method comprising: Step (1), add 10g of graphene to 40ml and vibrate ultrasonically for 10 minutes; Step (2), pouring the solid-liquid mixture of graphene and anhydrous ethanol into a ball mill for grinding and dispersion; Step (3), immersing the carbon fiber cloth to be used in a mixed solution of acetone and anhydrous ethanol in a ratio of 1:1 for 24 hours to remove impurities and sizing agents on the surface of the carbon fiber; Step (4), drying the cleaned carbon fiber cloth at 80 degrees Celsius, and then immersing it in concentrated nitric acid for 2 hours for ultrasonic oxidation treatment; Step (5), taking the graphene dispersion, spraying it evenly on the carbon fiber cloth to be used, and drying it in an oven at 80 degrees Celsius for standby use, to obtain the carbon fiber cloth containing graphene; Step (6), weighing epoxy resin, mixing epoxy resin and curing agent at a ratio of 100:20, and stirring evenly; Step (7), applying epoxy resin with curing agent added orthogonally to the front and back sides of the treated carbon fiber cloth, and stacking them one by one; In step (8), after standing at room temperature for half an hour, pressurizing and curing for 6 hours to prepare a carbon fiber / epoxy resin composite material containing graphene.
[0005] In one possible implementation, the grinding and dispersion in step (2) is performed for 2 hours to prepare a graphene suspension with a concentration of 1 mg / ml.
[0006] In a possible implementation, in step (6), a certain amount of prepared graphene-containing carbon fiber cloth is taken, and epoxy resin is weighed at a ratio of carbon fiber cloth to resin of 6:4.
[0007] In one possible implementation, in step (7), eight layers of carbon fiber cloth are laid down in succession.
[0008] Compared with the prior art, the present invention has the following beneficial effects: The method for preparing the graphene carbon fiber composite material of the embodiment of the present disclosure comprises weighing a certain amount of graphene, adding 40 ml of anhydrous ethanol, ultrasonicating for 10 minutes, then pouring the solid-liquid mixture of graphene and anhydrous ethanol into a ball mill and grinding and dispersing for 2 hours to prepare a graphene suspension with a concentration of 1 mg / ml. To remove impurities and sizing agents on the surface of the carbon fiber, the carbon fiber cloth to be used is immersed in a mixed solution of acetone and anhydrous ethanol (ratio 1:1) for 24 hours. The cleaned carbon fiber cloth is then dried at 80°C and then immersed in concentrated nitric acid for 2 hours for oxidation. Finally, a certain amount of graphene dispersion is taken and evenly sprayed on the carbon fiber cloth to be used, and then dried in an oven at 80°C for use, thereby producing a carbon fiber cloth containing a certain amount of graphene.
[0009] Take a certain amount of prepared graphene-containing carbon fiber cloth and weigh the resin at a ratio of 6:4 by weight of carbon fiber cloth to resin. Epoxy resin and curing agent are mixed at a ratio of 100:20 and stirred evenly. Apply the curing agent-treated epoxy resin orthogonally to both sides of the treated carbon fiber cloth, stacking the layers one by one until eight layers are laid. After standing at room temperature for half an hour, press-cure for 6 hours to produce a carbon fiber / epoxy resin composite.
[0010] Graphene was deposited onto the surface of carbon fibers to prepare a graphene-carbon fiber / epoxy resin composite. Mechanical and thermal properties were analyzed to determine the optimal graphene content. A graphene content of 0.2 wt% exhibited optimal performance, with interfacial shear strength increasing by 67.07%, interlaminar shear strength by 64.60%, flexural strength by 32.39%, and impact toughness by 41.97%.
[0011] A simpler and more effective method was adopted to incorporate graphene into the interface of carbon fiber-reinforced epoxy resin composites. The graphene was prepared into a dispersion, sprayed onto the carbon fiber cloth surface, and then epoxy resin was added for curing. This method effectively controlled the graphene content in the composite while avoiding the complex process of dispersing the graphene in the resin. BRIEF DESCRIPTION OF THE DRAWINGS
[0012] Figure 1 A graph showing the test results of the effect of graphene content on interface shear strength.
[0013] Figure 2 A graph showing the test results of the effect of graphene content on interlaminar shear strength.
[0014] Figure 3 A graph showing the test results of the effect of graphene content on the flexural strength of the composite material.
[0015] Figure 4 A graph showing the test results of the effect of graphene content on the impact toughness of composite materials.
[0016] Figure 5 A flowchart of a method for preparing a graphene carbon fiber composite material is shown. DETAILED DESCRIPTION
[0017] Various exemplary embodiments, features, and aspects of the present disclosure will be described in detail below with reference to the accompanying drawings. The same reference numerals in the accompanying drawings represent elements with the same or similar functions. Although various aspects of the embodiments are shown in the accompanying drawings, the drawings are not necessarily drawn to scale unless otherwise indicated.
[0018] The word “exemplary” is used exclusively herein to mean “serving as an example, example, or illustration.” Any embodiment described herein as “exemplary” is not necessarily to be construed as preferred or advantageous over other embodiments.
[0019] In addition, numerous specific details are provided in the following detailed description to better illustrate the present disclosure. Those skilled in the art will appreciate that the present disclosure can be practiced without certain specific details. In some instances, methods, means, components, and circuits well known to those skilled in the art are not described in detail in order to highlight the main points of the present disclosure.
[0020] According to one aspect of the present disclosure, Figure 5 As shown, a method for preparing a graphene carbon fiber composite material is provided, the method comprising: Step (1), add 10g of graphene to 40ml and vibrate ultrasonically for 10 minutes; Step (2), pouring the solid-liquid mixture of graphene and anhydrous ethanol into a ball mill for grinding and dispersion; Step (3), immersing the carbon fiber cloth to be used in a mixed solution of acetone and anhydrous ethanol in a ratio of 1:1 for 24 hours to remove impurities and sizing agents on the surface of the carbon fiber; Step (4), drying the cleaned carbon fiber cloth at 80 degrees Celsius, and then immersing it in concentrated nitric acid for 2 hours for ultrasonic oxidation treatment; Step (5), taking the graphene dispersion, spraying it evenly on the carbon fiber cloth to be used, and drying it in an oven at 80 degrees Celsius for standby use, to obtain the carbon fiber cloth containing graphene; Step (6), weighing epoxy resin, mixing epoxy resin and curing agent at a ratio of 100:20, and stirring evenly; Step (7), applying epoxy resin with curing agent added orthogonally to the front and back sides of the treated carbon fiber cloth, and stacking them one by one; In step (8), after standing at room temperature for half an hour, pressurizing and curing for 6 hours to prepare a carbon fiber / epoxy resin composite material containing graphene.
[0021] Graphene was deposited onto the surface of carbon fibers to prepare a graphene-carbon fiber / epoxy resin composite. Mechanical and thermal properties were analyzed to determine the optimal graphene content. A graphene content of 0.2 wt% exhibited optimal performance, with interfacial shear strength increasing by 67.07%, interlaminar shear strength by 64.60%, flexural strength by 32.39%, and impact toughness by 41.97%.
[0022] A simpler and more effective method was adopted to incorporate graphene into the interface of carbon fiber-reinforced epoxy resin composites. The graphene was prepared into a dispersion, sprayed onto the carbon fiber cloth surface, and then epoxy resin was added for curing. This method effectively controlled the graphene content in the composite while avoiding the complex process of dispersing the graphene in the resin.
[0023] In one possible implementation, the grinding and dispersion in step (2) is performed for 2 hours to prepare a graphene suspension with a concentration of 1 mg / ml.
[0024] In a possible implementation, in step (6), a certain amount of prepared graphene-containing carbon fiber cloth is taken, and epoxy resin is weighed at a ratio of carbon fiber cloth to resin of 6:4.
[0025] In one possible implementation, in step (7), eight layers of carbon fiber cloth are laid down in succession.
[0026] The interface shear strength test can directly reflect the interface bonding strength between carbon fiber and epoxy resin. The interface shear strength test results can be used to determine the effect of graphene on the carbon fiber-epoxy resin interface. The interface shear strength test results with different graphene contents are as follows: Figure 1As shown. With the increase of graphene content on the carbon fiber surface, the interfacial shear strength changes significantly. In addition, with the increase of graphene content, the interfacial shear strength first increases and then decreases. When the graphene content is 0.1 wt%, a small amount of graphene is attached to the carbon fiber surface, which slightly improves the interfacial shear strength between the carbon fiber and the epoxy resin. With the increase of graphene content, when the graphene content is 0.2 wt%, the interfacial shear strength reaches 66.92 MPa, which is 67.07% higher than that of the carbon fiber without graphene. However, when the graphene content exceeds 0.2 wt%, the interfacial shear strength decreases slightly. This is attributed to the agglomeration of a large amount of graphene on the carbon fiber surface and the stress concentration site, which hinders energy transfer and leads to a decrease in interfacial strength. The interfacial shear strength of the composite material with 1 wt% graphene decreases to 41.18 MPa, which further proves that graphene aggregation causes a decrease in interfacial properties.
[0027] Effect of graphene content on interlaminar shear strength of carbon fiber reinforced epoxy resin matrix composites Figure 2 As shown. Figure 2 It can be seen that the addition of a small amount of graphene significantly improves the interlaminar shear strength of the composite material, and as the graphene content increases, the shear strength first increases and then decreases. When the graphene content is 0.2 wt%, it reaches a maximum of 37.26 MPa, a 64.60% increase compared to the blank sample. This is because the addition of an appropriate amount of graphene improves the wettability and mechanical bite between the epoxy resin and the carbon fiber, thereby significantly improving the interfacial bonding strength. When the addition reaches 1 wt%, the shear strength drops to 20.93 MPa, which is lower than the strength of the composite material without graphene.
[0028] To further investigate the enhancement of the interfacial properties by graphene, we investigated the flexural properties of the composites. Figure 3 As shown. Figure 3As can be seen from the graphene content, both the flexural strength and flexural modulus of the composite material are significantly improved. The flexural strength gradually increases with increasing graphene content, reaching its highest strength at 0.2 wt% and then decreasing with increasing graphene content. Compared to the composite without graphene, the flexural strength of the carbon fiber reinforced resin matrix composite with 0.2 wt% graphene increased by 31.84% and the flexural modulus by 23.94%. The variation in the flexural strength of the composite material is consistent with the interfacial shear strength and interlaminar shear strength, indicating a strong correlation between the flexural strength and interfacial strength. When the graphene content exceeds 0.2 wt%, the flexural strength and modulus of the composite material decrease, showing a similar trend to the interlaminar shear strength. This is because the introduction of graphene creates a stronger interface between the carbon fiber and epoxy resin, resulting in better stress transfer from the epoxy matrix to the carbon fiber. However, excessive graphene can aggregate at the interface, creating new stress concentration sites and reducing the flexural strength.
[0029] As the graphene content increases, the impact toughness of the composite material shows a trend of first increasing and then decreasing, which is similar to the interlaminar shear strength and bending strength. Figure 4 As shown in Figure 3 , with increasing graphene content, the composite material shows a trend of first increasing and then decreasing, similar to the interlaminar shear strength and flexural strength. The impact toughness of the carbon fiber epoxy resin-based composite increases from 16.18±1.65 kJ / m² to 22.97±1.36 kJ / m², increasing by approximately 41.97% when the graphene content is 0.2 wt%, and then decreasing slightly. The effects of graphene on the three aforementioned mechanical properties of carbon fiber composites tend to be similar, initially increasing and then decreasing, with the enhancement effect being optimal at a content of 0.2 wt%.
[0030] While various embodiments of the present disclosure have been described above, the foregoing description is intended to be illustrative, non-exhaustive, and not limited to the disclosed embodiments. Many modifications and variations will be apparent to those skilled in the art without departing from the scope and spirit of the described embodiments. The terminology used herein is selected to best explain the principles of the embodiments, their practical applications, or technological improvements in the marketplace, or to enable others skilled in the art to understand the embodiments disclosed herein.
Claims
1. A method for preparing a graphene carbon fiber composite material, characterized in that: The method comprises: Step (1), add 10g of graphene to 40ml and vibrate ultrasonically for 10 minutes; Step (2), pouring the solid-liquid mixture of graphene and anhydrous ethanol into a ball mill for grinding and dispersion; Step (3), immersing the carbon fiber cloth to be used in a mixed solution of acetone and anhydrous ethanol in a ratio of 1:1 for 24 hours to remove impurities and sizing agents on the surface of the carbon fiber; Step (4), drying the cleaned carbon fiber cloth at 80 degrees Celsius, and then immersing it in concentrated nitric acid for 2 hours for ultrasonic oxidation treatment; Step (5), taking the graphene dispersion, spraying it evenly on the carbon fiber cloth to be used, and drying it in an oven at 80 degrees Celsius for standby use, to obtain the carbon fiber cloth containing graphene; Step (6), weighing epoxy resin, mixing epoxy resin and curing agent at a ratio of 100:20, and stirring evenly; Step (7), applying epoxy resin with curing agent added orthogonally to the front and back sides of the treated carbon fiber cloth, and stacking them one by one; In step (8), after standing at room temperature for half an hour, pressurizing and curing for 6 hours to prepare a carbon fiber / epoxy resin composite material containing graphene.
2. The method for preparing a graphene carbon fiber composite material according to claim 1, wherein: In step (2), the graphene suspension was prepared by grinding and dispersing for 2 hours to a concentration of 1 mg / ml.
3. The method for preparing a graphene carbon fiber composite material according to claim 1, wherein: In step (6), a certain amount of prepared graphene-containing carbon fiber cloth is taken, and epoxy resin is weighed according to a ratio of carbon fiber cloth to resin of 6:
4.
4. The method for preparing a graphene carbon fiber composite material according to claim 1, wherein: In step (7), eight layers of carbon fiber cloth are laid one by one.