Preparation method of three-dimensional graphene carbon fiber composite board
By adding three-dimensional graphene to the carbon fiber composite material, a three-dimensional graphene carbon fiber composite laminate with significantly improved damping performance was prepared, which solved the problem of poor damping performance of carbon fiber composite material and achieved better vibration damping effect.
Patent Information
- Application Number
- CN202411563388.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-05
- Publication Date
- 2025-02-14
AI Technical Summary
The high stiffness of carbon fiber composite materials leads to poor damping performance, which leads to the structure prone to tiny cracks when it vibrates, which leads to premature failure of the components.
By adding three-dimensional graphene to the carbon fiber composite material, a three-dimensional graphene carbon fiber composite laminate is prepared by chemical vapor deposition method to enhance its damping performance.
The damping performance of carbon fiber composite laminated plates was significantly improved, with the modal damping ratio increased from 3.03% to 6.72%, and the resonance amplitude was lower than that of the raw material, indicating that it had better damping effect on vibration.
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Figure CN119427781A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to a method for preparing a carbon fiber composite plate, and in particular to a method for preparing a three-dimensional graphene carbon fiber composite plate. Background Art
[0002] In recent years, advanced composite materials represented by carbon fiber reinforced resin-based composite materials have the advantages of high specific strength, specific modulus, excellent manufacturability, fatigue resistance, corrosion resistance, etc., and are gradually replacing traditional metal materials and are increasingly used in various fields. However, the high stiffness of carbon fiber composite materials means low damping performance, and the structures prepared by them have poor vibration resistance, which causes small cracks in these structures to expand rapidly and premature failure of components. Therefore, improving the damping performance of carbon fiber composite materials has become a current research hotspot.
[0003] Three-dimensional graphene has a unique three-dimensional porous network structure, which brings a lot of interface slip and increases the energy dissipation of the composite material, thus showing excellent damping and vibration reduction performance. Compared with two-dimensional graphene, it is less likely to agglomerate and stack, which is conducive to maintaining the performance stability of the material. Therefore, the damping performance of carbon fiber composites enhanced with three-dimensional graphene has attracted widespread attention. Summary of the invention
[0004] The object of the present invention is to provide a method for preparing a three-dimensional graphene carbon fiber composite plate, wherein the modal damping ratio of the carbon fiber composite laminate to which the three-dimensional graphene is added is 6.72%, indicating that the three-dimensional graphene can enhance the damping performance of the carbon fiber composite laminate. By testing the modal damping ratio of the carbon fiber composite laminate, under the action of the three-dimensional graphene, the damping performance of the three-dimensional graphene carbon fiber composite laminate is significantly improved.
[0005] The objective of the present invention is achieved through the following technical solutions: A method for preparing a three-dimensional graphene carbon fiber composite plate, the method comprising the following steps: Step S1, placing nickel foam with a thickness of 2 mm in acetone and distilled water for ultrasonic treatment for 30 minutes; Step S2, then put it into an oven at 50°C and dry it for 5 hours; Step S3, placing the nickel foam in the center of the tube furnace and setting the three-dimensional graphene growth parameters; Step S4, introducing 200 sccm of Ar and 100 sccm of H2 and starting the tubular furnace heating system; Step S5, after the temperature of the tubular furnace is raised to 1000° C., the nickel foam is annealed for 30 minutes; Step S6, introducing 25 sccm of CH4 gas for 35 min; Step S7, the cooled graphene-nickel hybrid three-dimensional foam material is placed in a FeCl3 mixed solution for etching; Step S8, after etching, washing with distilled water and drying in an oven at 80°C to obtain three-dimensional graphene; Step S9, placing a hard glass plate cleaned with acetone on the workbench; Step S10, after applying a layer of release agent evenly on the glass plate, stack the pre-cut carbon fiber cloth neatly, a total of 4 layers, and place them in the center of the glass plate; Step S11, adding three-dimensional graphene in the middle of the carbon fiber cloth; Step S12: Next, use a sealing rubber ring to circle out an area of about 25 cm × 15 cm; Step S13, placing two liquid guide tubes at a distance of 2 cm from the left and right ends of the carbon fiber cloth, respectively, setting T-shaped three-way joints on the connection ports at the tops of the two sections of the guide tubes embedded with sealant, and then horizontally sleeve the liquid guide tubes separately; Step S14, compacting the plastic isolation film with a roller to prevent air bubbles from leaking and damaging the sealing performance; Step S15, placing the vacuum-assisted mold on a heating table, and setting the temperature of the heating table to 100° C.; Step S16, connecting the sealed mold to the vacuum equipment through one end of the guide tube; Step S17, immersing the other end in a mixed solution of epoxy resin and curing agent; Step S18, start the vacuum pump to extract the excess gas in the mold, and pour the epoxy resin and curing agent mixed solution into the mold under the action of vacuum pressure; Step S19, after the epoxy resin and curing agent mixed solution are completely poured, clamp the two ends of the mold with a clamp to ensure that the mold is airtight and put it into the oven; Step S20, setting the oven temperature at 100°C for curing for 4 hours, 140°C for curing for 4 hours, and 180°C for curing for 4 hours; Step S21, obtaining a three-dimensional graphene carbon fiber composite laminate after curing; The three-dimensional graphene carbon fiber composite material laminate preparation method is described, wherein the three-dimensional graphene is based on a nickel foam with a thickness of 2 mm and is prepared by chemical vapor deposition.
[0006] In the method for preparing a three-dimensional graphene carbon fiber composite laminate, the epoxy resin is one or more of E51 epoxy resin, 618 epoxy resin, and 128 epoxy resin.
[0007] In the method for preparing a three-dimensional graphene carbon fiber composite laminate, the curing agent is one or more of W93 curing agent and Q593 curing agent.
[0008] The advantages and effects of the present invention are: The present invention tests the modal damping ratio of carbon fiber composite laminates. Under the action of three-dimensional graphene, the damping performance of the three-dimensional graphene carbon fiber composite laminates is improved, and the modal damping ratio of the carbon fiber composite laminates with three-dimensional graphene added is 6.72%, which shows that three-dimensional graphene can enhance the damping performance of carbon fiber composite laminates.
[0009] The specimens were tested by hammering method. The results showed that the modal damping ratio of the carbon fiber composite laminate was 3.03%, and the modal damping ratio of the three-dimensional graphene carbon fiber composite laminate was 6.72%. Compared with the carbon fiber composite laminate, the modal damping ratio of the three-dimensional graphene carbon fiber composite laminate was increased by 122%. The resonance amplitude of the three-dimensional graphene carbon fiber composite laminate was lower than that of the carbon fiber composite laminate. The resonance amplitude of the three-dimensional graphene carbon fiber composite laminate was lower than that of the carbon fiber composite laminate, indicating that its corresponding vibration damping ratio was higher than that of the carbon fiber composite laminate, which was consistent with the experimental results measured by hammering method. Compared with the carbon fiber composite laminate, the modal damping ratio of the carbon fiber composite laminate with three-dimensional graphene was improved. BRIEF DESCRIPTION OF THE DRAWINGS
[0010] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art are briefly introduced below. Obviously, for those skilled in the art, other drawings can be obtained based on these drawings without paying any creative work.
[0011] Figure 1 It is a schematic diagram of the flow chart of the present invention; Figure 2 Provide a physical picture of a three-dimensional graphene growth tube furnace for Example 1 of the present invention; Figure 3 Provides a photograph of graphene-nickel hybrid three-dimensional foam material etched in FeCl3 solution for Example 1 of the present invention; Figure 4 Provide a photo of three-dimensional graphene for Example 1 of the present invention; Figure 5 This is a vacuum-assisted mold diagram of a laminate of Example 1 of the present invention; Figure 6 Provide a vacuum assisted resin transfer molding diagram for Example 1 of the present invention; Figure 7 Provide a photo of a three-dimensional graphene carbon fiber composite laminate for Example 1 of the present invention; Figure 8Provide the first-order modal vibration shape diagram of a carbon fiber composite laminate and a three-dimensional graphene carbon fiber composite laminate for Example 1 of the present invention; Fig. 9 Provide a second-order modal vibration shape diagram of a carbon fiber composite laminate and a three-dimensional graphene carbon fiber composite laminate for Example 1 of the present invention; Fig.10 Provide the third-order modal vibration shape diagram of the carbon fiber composite laminate and the three-dimensional graphene carbon fiber composite laminate for Example 1 of the present invention; Fig.11 Provide a 4th-order modal vibration shape diagram of a carbon fiber composite laminate and a three-dimensional graphene carbon fiber composite laminate for Example 1 of the present invention; Fig.12 A comparison diagram of the first-order response amplitudes of a carbon fiber composite laminate and a three-dimensional graphene carbon fiber composite laminate is provided for Example 1 of the present invention. DETAILED DESCRIPTION
[0012] In order to enable those skilled in the art to better understand the technical solutions in the present invention, the technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative work should fall within the protection scope of the present invention. Example 1
[0013] The preparation process of the three-dimensional graphene carbon fiber composite laminate of the present invention is as follows: Figure 1 As shown, the method comprises the following steps: The nickel foam was ultrasonically placed in acetone and distilled water for 30 minutes, and then placed in an oven for drying. The nickel foam was placed in the center of the tube furnace and the three-dimensional graphene growth parameters were set. After the tube furnace was heated to 1000°C, the nickel foam was annealed for 30 minutes, and then CH4 gas was introduced for 35 minutes. The cooled graphene nickel hybrid three-dimensional foam material was placed in a FeCl3 mixed solution for etching, and after etching, it was washed with distilled water and placed in an 80°C oven for drying to obtain three-dimensional graphene. A hard glass plate (size 30cm×30cm, thickness 0.4cm) washed with acetone was placed on the workbench. After evenly applying a layer of release agent on the glass plate, the pre-cut carbon fiber cloth (size 15cmx5cm) was neatly stacked and placed in the center of the glass plate for a total of 4 layers, and three-dimensional graphene was added in the middle of the carbon fiber cloth. Next, a sealant was used to circle an area of about 25cm×15cm, and the plastic isolation film was compacted with a roller to prevent the presence of bubbles from causing air leakage and destroying the sealing. Then connect the sealed mold to the vacuum equipment through one end of the guide tube, and immerse the other end in the mixed solution of epoxy resin and curing agent; turn on the vacuum pump to extract the excess gas in the mold, and pour the mixed solution of epoxy resin and curing agent into the mold under the action of vacuum pressure. In this process, it is necessary to pay attention to controlling the flow rate of epoxy resin to ensure that the mixed solution of epoxy resin and curing agent completely infiltrates the composite material. Finally, after the mixed solution of epoxy resin and curing agent is completely poured, use a clamp to clamp the two ends of the mold to ensure that the mold is airtight and put it into the oven. Set the oven temperature to cure for 4 hours at 100℃, 4 hours at 140℃, and 4 hours at 180℃, and finally obtain a three-dimensional graphene carbon fiber composite laminate.
[0014] Table 1 The first-order natural frequency and modal damping ratio of carbon fiber composite laminates Three-dimensional graphene Order Natural frequency / Hz Modal damping ratio / % have 1 33.3 6.72 none 1 30.6 3.03 The prepared three-dimensional graphene carbon fiber composite laminate is as follows Figure 7As shown. This scheme tests the three-dimensional graphene carbon fiber composite laminate and the carbon fiber composite laminate by the hammer method. After adding three-dimensional graphene, the damping performance of the carbon fiber composite laminate is improved. Referring to Table 1, the modal damping ratio of the carbon fiber composite laminate is 3.03%, and the modal damping ratio of the three-dimensional graphene carbon fiber composite laminate is 6.72%. Compared with the carbon fiber composite laminate, the modal damping ratio of the three-dimensional graphene carbon fiber composite laminate is increased by 122%. The resonance amplitude of the three-dimensional graphene carbon fiber composite laminate is lower than that of the carbon fiber composite laminate. The resonance amplitude of the three-dimensional graphene carbon fiber composite laminate is lower than that of the carbon fiber composite laminate, indicating that its corresponding vibration damping ratio is higher than that of the carbon fiber composite laminate, which is consistent with the experimental results measured based on the hammer method. Compared with the carbon fiber composite laminate, the modal damping ratio of the carbon fiber composite laminate with the addition of three-dimensional graphene is improved.
[0015] In order to enable those skilled in the art to better understand the technical solutions in the present invention, the technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative work should fall within the protection scope of the present invention.
Claims
1. A method for preparing a three-dimensional graphene carbon fiber composite plate, characterized in that: The method comprises the following preparation steps: Step S1, placing nickel foam with a thickness of 2 mm in acetone and distilled water for ultrasonic treatment for 30 minutes; Step S2, then put it into an oven at 50°C and dry it for 5 hours; Step S3, placing the nickel foam in the center of the tube furnace and setting the three-dimensional graphene growth parameters; Step S4, introducing 200 sccm of Ar and 100 sccm of H2 and starting the tubular furnace heating system; Step S5, after the temperature of the tubular furnace is raised to 1000° C., the nickel foam is annealed for 30 minutes; Step S6, introducing 25 sccm of CH4 gas for 35 min; Step S7, the cooled graphene-nickel hybrid three-dimensional foam material is placed in a FeCl3 mixed solution for etching; Step S8, after etching, washing with distilled water and drying in an oven at 80°C to obtain three-dimensional graphene; Step S9, placing a hard glass plate cleaned with acetone on the workbench; Step S10, after applying a layer of release agent evenly on the glass plate, stack the pre-cut carbon fiber cloth neatly, a total of 4 layers, and place them in the center of the glass plate; Step S11, adding three-dimensional graphene in the middle of the carbon fiber cloth; Step S12: Next, use a sealing rubber ring to circle out an area of about 25 cm × 15 cm; Step S13, placing two liquid guide tubes at a distance of 2 cm from the left and right ends of the carbon fiber cloth, respectively, setting T-shaped three-way joints on the connection ports at the tops of the two sections of the guide tubes embedded with sealant, and then horizontally sleeve the liquid guide tubes separately; Step S14, compacting the plastic isolation film with a roller to prevent air bubbles from leaking and damaging the sealing performance; Step S15, placing the vacuum-assisted mold on a heating table, and setting the temperature of the heating table to 100° C.; Step S16, connecting the sealed mold to the vacuum equipment through one end of the guide tube; Step S17, immersing the other end in a mixed solution of epoxy resin and curing agent; Step S18, start the vacuum pump to extract the excess gas in the mold, and pour the epoxy resin and curing agent mixed solution into the mold under the action of vacuum pressure; Step S19, after the epoxy resin and curing agent mixed solution are completely poured, clamp the two ends of the mold with a clamp to ensure that the mold is airtight and put it into the oven; Step S20, setting the oven temperature at 100°C for curing for 4 hours, 140°C for curing for 4 hours, and 180°C for curing for 4 hours; Step S21, after curing, a three-dimensional graphene carbon fiber composite laminate is obtained.
2. The method for preparing a three-dimensional graphene composite plate according to claim 1, characterized in that: The three-dimensional graphene is prepared by chemical vapor deposition using nickel foam with a thickness of 2 mm as a substrate.
3. The method for preparing a three-dimensional graphene composite plate according to claim 1, characterized in that: The epoxy resin is one or more of E51 epoxy resin, 618 epoxy resin and 128 epoxy resin.
4. The method for preparing a three-dimensional graphene composite plate according to claim 1, characterized in that: The curing agent is one or more of W93 curing agent and Q593 curing agent.
5. The method for preparing a three-dimensional graphene composite plate according to claim 1, characterized in that: The epoxy resin and curing agent were mixed uniformly by mechanical stirring and ultrasonic dispersion for 30 min.